Dess-Martin periodinane CAS 87413-09-0

Introduction:Basic information about Dess-Martin periodinane CAS 87413-09-0, including its chemical name, molecular formula, synonyms, physicochemical properties, and safety information, etc.

Dess-Martin periodinane Basic information

Product Name:Dess-Martin periodinane
Synonyms:Dess-Martin periodinane,D M P, TAPI;dess-martin periodinate;1,1,1-Triacetoxy-1,2-benziodoxole-IV-3(1H)-one;1,1,1-Triacetoxy-1,3-dihydro-3-oxo-1,2-benziodoxole-IV;1,1,1-Triacetoxy-3H-1,2-benziodoxole-IV-3-one;Martin's reagent;1,1-Dihydro-1,1,1-triacetoxy-1,2-benzoiodooxol-3(1H)-one (Dess-M;Dess-Martin periodinane solution
CAS:87413-09-0
MF:C13H13IO8
MW:424.14
EINECS:672-328-8
Product Categories:Hypervalent Iodine;Synthetic Reagents;Hypervalent Iodine Compounds;Oxidation;Synthetic Organic Chemistry;Fused Ring Systems
Mol File:87413-09-0.mol

Dess-Martin periodinane Chemical Properties

Melting point 130-133 °C (lit.)
Boiling point 40 °C
density 1.369 g/mL at 25 °C
Fp >221 °F
storage temp. -20°C
solubility Soluble in chloroform, acetone, acetonitrile and methylene chloride. Slightly soluble in ether and hexane.
form Liquid
color Colorless to light yellow
Sensitive Light Sensitive
Merck 14,2933
BRN 4548207
Stability:Light Sensitive
InChIInChI=1S/C13H13IO8/c1-8(15)19-14(20-9(2)16,21-10(3)17)12-7-5-4-6-11(12)13(18)22-14/h4-7H,1-3H3
InChIKeyNKLCNNUWBJBICK-UHFFFAOYSA-N
SMILESI1(OC(=O)C)(OC(=O)C)(OC(=O)C)OC(=O)C2C=CC=CC1=2
CAS DataBase Reference87413-09-0(CAS DataBase Reference)

Safety Information

Hazard Codes Xn,O,Xi
Risk Statements 22-36/37/38-40-8-20/21/22-44
Safety Statements 26-36-36/37-24/25-23-17-45-36/37/39
RIDADR UN 1593 6.1/PG 3
WGK Germany 3
Hazard Note Harmful/Light sensitive
TSCA No
HazardClass 5.1
PackingGroup 
HS Code 29349990
Storage Class5.2 - Organic peroxides and self-reacting hazardous materials
Hazard ClassificationsEye Irrit. 2
Self-react. C
Skin Irrit. 2
STOT SE 3

Dess-Martin periodinane Usage And Synthesis

DescriptionDess-Martin periodinane (DMP) is a hypervalent iodine compound widely used as a mild reagent for the oxidation of primary/secondary alcohols to aldehydes/ketones; oxidation of amides into imides; the dehydrogenation of amines to nitriles, and disulfides to sulfones. It is also used to selectively oxidize alkenes to epoxides. This is a useful reaction for generating three-membered cyclic ethers. Additionally, DMP is used to oxidatively cleave 1,2-diols to form aldehydes or ketones and in the synthesis of lactones.
Chemical PropertiesWhite Crystalline powder
UsesDess-Martin Periodinaneis a very usefulreagent used in the oxidation of primary alcohols to aldehydes and secondary alcohols to ketones.
UsesOxidizing reagent.
UsesDess Martin periodinane is used to oxidize primary alcohols to aldehydes and secondary alcohols to ketones. It is also used as an oxidant for complexes with multifunctional alcohols. It is actively involved in the oxidation of N-protected-amino alcohols without epimerization and allylic alcohols.
reaction suitabilityreagent type: oxidant
Synthesis

2-Iodobenzoic acid (50.0 g,0.20 mol) was added to cyclobutanesulfone (250 mL), and the solution was heated to 50 ??C. 90% of the above solution was slowly added dropwise to an aqueous solution of potassium persulfate (147.4g,0.24mol,1.2eq) at 50??C (300mL) and the reaction was held for 3 hours. Subsequently, the reaction solution was heated to 95 ??C and the remaining 10% 2-iodobenzoic acid solution was slowly added dropwise to the reaction solution and the reaction was continued for 3 hours. Upon completion of the reaction, the reaction was cooled to 5 ??C and stirring was continued at this temperature for 1.5 hours. Under stirring, 1 L of water was added, filtered (the filtrate was to be recycled for set use), the filter cake was washed with water and acetone sequentially, and dried at room temperature for 16 hours to obtain 53.2 g of 2-iodobenzoic acid (yield 95.04%), white solid, with a purity of 99.7% (confirmed by NMR and HPLC). The solid was identified as 2-iodoacylbenzoic acid by HNMR.

2-Iodoacylbenzoic acid (45 g, 0.16 mol) was added to acetic anhydride (49 g, 0.48 mol) and dioxane (90 mL), followed by B(C6F5)3 (0.0016 mol) followed by B(C6F5)3 (0.0016 mol), and the reaction solution was heated to 50 ??C and stirred for 10 min, then the solvent was evaporated off by spin-drying under reduced pressure, and the reaction solution was added to methyl tert-butyl ether (400 mL). Filtered and dried at room temperature to obtain a white solid (61.1 g, yield: 90%). The purity of Desmartin oxidizer was 99.1% (confirmed by NMR).

AdvantagesBenefits of using Dess-Martin periodinane (DMP) as an oxidizing reagent:
milder reaction conditions (room temperature, neutral pH)
shorter reaction times and higher yields
high chemoselectivity
tolerance of sensitive functional groups, and a long shelf life
simplified workups

Dess-Martin periodinane Preparation Products And Raw materials

Raw materialsAcetic acid-->Acetic anhydride-->p-Toluenesulfonic acid-->Potassium bromate-->2-Iodobenzoic acid-->2-Iodoxybenzoic acid
Preparation ProductsC-(3,4-DIHYDRO-2H-BENZO[1,4]OXAZIN-3-YL)-METHYLAMINE-->3-Chloro-4-Cyanobenzaldehyde-->3-(4-FLUORO-PHENYL)-1-ISOPROPYL-1H-INDOLE-2-CARBALDEHYDE-->(3-OXO-PROPYL)-CARBAMIC ACID TERT-BUTYL ESTER-->4-FORMYL-N-CBZ-PIPERIDINE-->1-[[(4-METHYLPHENYL)SULPHONYL]OXY]-1,2-BENZIODOXOL-3(1H)-ONE-->1H-Indazole-1-propanoic acid
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