Ethanethiol → HCID 53629164, 화합물

HRID 1896389노트

반응식

HRID 1896389 반응식
[C:1]([C:3]1[N:4]=[CH:5][N:6]([CH3:11])[C:7]=1[C:8](O)=[O:9])#[N:2].[CH2:12]([SH:14])[CH3:13].C1CCC(N=C=NC2CCCCC2)CC1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[C:1]([C:3]1[N:4]=[CH:5][N:6]([CH3:11])[C:7]=1[C:8](=[O:9])[S:14][CH2:12][CH3:13])#[N:2]

참가 물질

6

반응물 3

HCID 6343Ethanethiol2회HCID 10868DicyclohexylcarbodiimideHCID 450820154-Cyano-1-methyl-1H-imidazole-5-carboxylic acid

생성물 1

HCID 53629164HCID 53629164, 화합물수율 93.3%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

In a 1 l, three-necked flask fitted with a magnetic stirrer and a reflux condenser under inert atmosphere, 4-cyano-1-methyl-1H-imidazole-5-carboxylic acid x84 (24.5 g, 0.162 mol) and CH2Cl2 (500 ml) are stirred at room temperature. To this suspension, ethanethiol (13.2 ml, 0.178 mol) and DMAP (1.98 g, 0.016 mol) are added, followed by DCC (36.77 g, 0.178 mol) in two portions. The temperature rises to 35° C. and the mixture is stirred at room temperature for 16 h. Ethanethiol (0.0324 mol) is further added and stirring is continued overnight. The mixture is filtered and the solvent is evaporated. The residue is purified by chromatography on silicagel (Hexane/AcOEt: 6/4 (v/v)) to give 29.5 g of S-ethyl 4-cyano-1-methyl-1H-imidazole-5-carbothioate x85.

후처리

  1. customrises to 35° C.
  2. stirringthe mixture is stirred at room temperature for 16 h
  3. stirringstirring
  4. filtrationThe mixture is filtered
  5. customthe solvent is evaporated
  6. customThe residue is purified by chromatography on silicagel (Hexane/AcOEt: 6/4 (v/v))

출처 및 근거

ORD 기록
ord-03ae3ef13fbd42528be0d4dd6bee2109
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518943B2

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