Methylamine → HCID 57461305、化合物

HRID 1994361ノート

反応式

HRID 1994361 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-53cb03da43f54d24a41e92dca11d6a17
出典データセット
uspto-grants-2010_01
特許番号
US07652150B2

反応ノート

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