Methylamine → N-methyl benzothiophene-2-carboxamide

HRID 1921020

反応式

HRID 1921020 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-47d206de047e4ee68e496aeaa0acb160
出典データセット
uspto-grants-2012_05
特許番号
US08173646B2

関連ノート

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