Methylamine → HCID 57461305、化合物

HRID 16636ノート

反応式

HRID 16636 の反応式
[C:1](N1C=CN=C1)([N:3]1C=CN=C1)=O.[NH:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]([S:22][C:23]2[CH:31]=[CH:30][CH:29]=[CH:28][C:24]=2[C:25](O)=[O:26])=[CH:14]1.CN>C1COCC1>[NH:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]([S:22][C:23]2[CH:31]=[CH:30][CH:29]=[CH:28][C:24]=2[C:25]([NH:3][CH3:1])=[O:26])=[CH:14]1

参加物

5

反応物 3

HCID 6329MethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 107544492-(1H-indol-3-ylsulfanyl)benzoic Acid

生成物 1

HCID 57461305HCID 57461305、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Carbonyldiimidazole (11 mmol) was added to a solution of 2-(1H-indol-3-ylsulfanyl)benzoic acid (Hamel, P.; Girard, M.; Tsou, N. N.; J. Heterocycl. Chem. 36, 1999, 643-652) (10 mmol) in dry THF (200 mL) and refluxed for 60 minutes under argon. Methyl amine (1M in THF; 40 ml) was added slowly to the reaction mixture and the mixture was stirred at room temperature for 16 hours. The mixture was evaporated in vacuo and the product purified by column chromatography on silica gel using ethyl acetate as an eluent.

後処理

  1. temperaturerefluxed for 60 minutes under argon
  2. customThe mixture was evaporated in vacuo
  3. customthe product purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-6acc1c84317640eb986465cb801c97d5
出典データセット
uspto-grants-2010_06
特許番号
US07737171B2

反応ノート

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