Triethylamine → 3-(2-Methoxybenzamido)thiophene-2-carboxamide

HRID 333700

반응식

HRID 333700 반응식
[NH2:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]([NH2:9])=[O:8].CCN(CC)CC.CN(C1C=CC=CN=1)C.[CH3:26][O:27][C:28]1[CH:36]=[CH:35][CH:34]=[CH:33][C:29]=1[C:30](Cl)=[O:31]>C(Cl)Cl.O>[CH3:26][O:27][C:28]1[CH:36]=[CH:35][CH:34]=[CH:33][C:29]=1[C:30]([NH:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]([NH2:9])=[O:8])=[O:31]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 889692-Methoxybenzoyl chlorideHCID 5189933-Aminothiophene-2-carboxamide

생성물 1

HCID 590266413-(2-Methoxybenzamido)thiophene-2-carboxamide수율 80.4%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A solution of 3-aminothiophene-2-carboxamide (0.90 g, 6.3 mmol), Et3N (0.97 mL, 7.0 mmol), and dimethylaminopyridine (0.15 g, 1.3 mmol) in CH2Cl2 (21 mL) was cooled in an ice bath, and 2-methoxybenzoyl chloride (1.1 g, 6.3 mmol) was added dropwise. The reaction was stirred for 1 h, and water (20 mL) was added. The solids were filtered, washed with water, and dried under vacuum to give 3-(2-methoxybenzamido)thiophene-2-carboxamide (1.4 g, 79% yield). LC/MS: m/z 277.3 (M+H)+ at 2.61 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

후처리

  1. filtrationThe solids were filtered
  2. washwashed with water
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-e9da4b511b4b40488b3e67b40963f8f7
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883781B2

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