Methylamine → N-methyl benzothiophene-2-carboxamide

HRID 1710539

반응식

HRID 1710539 반응식
[CH3:1][NH2:2].[S:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH:5]=[C:4]1[C:12](Cl)=[O:13]>C1COCC1>[CH3:1][NH:2][C:12]([C:4]1[S:3][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH:5]=1)=[O:13]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 142384Benzo[b]thiophene-2-carbonyl Chloride

생성물 1

HCID 22593821N-methyl benzothiophene-2-carboxamide수율 98%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a stirred solution of 2.0 M methylamine in THF (60 mL) and THF (60 mL) was added dropwise at 0° C. a solution of benzothiophene-2-carbonyl chloride (10.8 g, 55 mmole) in THF (50 mL) over 15 minutes. After the addition the reaction was allowed to warm to RT then was concentrated under vacuum. Trituration with a cold solution of 4:1 H2O/methanol (50 mL), filtration, and drying under vacuum gave the title compound (10.35 g, 98%) as a white solid: MS (ES) m/e 191.9 (M+H)+.

후처리

  1. additionAfter the addition the reaction
  2. concentrationthen was concentrated under vacuum
  3. filtrationTrituration with a cold solution of 4:1 H2O/methanol (50 mL), filtration
  4. customdrying under vacuum

출처 및 근거

ORD 기록
ord-04ad0ef25d4946359456738379f4907a
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790716B2

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