Methylamine → N-methyl benzothiophene-2-carboxamide

HRID 1710539

反応式

HRID 1710539 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 22593821N-methyl benzothiophene-2-carboxamide収率 98%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-04ad0ef25d4946359456738379f4907a
出典データセット
uspto-grants-2010_09
特許番号
US07790716B2

関連ノート

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