Water → 7-Bromo-2-phenylthieno[3,2-c]pyridin-4(5H)-one

HRID 1868324ノート

反応式

HRID 1868324 の反応式
[C:1]1([C:7]2[S:15][C:14]3[CH:13]=[CH:12][NH:11][C:10](=[O:16])[C:9]=3[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1C(=O)N([Br:24])C(=O)C1.O>CN(C=O)C>[Br:24][C:13]1[C:14]2[S:15][C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[CH:8][C:9]=2[C:10](=[O:16])[NH:11][CH:12]=1

参加物

5

反応物 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 184465262-phenylthieno[3,2-c]pyridin-4(5H)-one

生成物 1

HCID 184465837-Bromo-2-phenylthieno[3,2-c]pyridin-4(5H)-one収率 96.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To compound 2 (3.92 g, 17.24 mmol) in DMF (133 mL) was added NBS (3.37 g, 19.0 mmol). The solution was heated to 60° C. After 1 h, the solution volume was reduced to approximately one half the volume, and the solution was poured into H2O (700 mL). The precipitate was filtered, washed with water, and dried to yield 5.08 g of 3. 1H NMR (400 MHz, d6-DMSO) δ: 11.84 (s, 1H), 8.05 (s, 1H), 7.82 (d, J=7 Hz, 2H), 7.61 (s, 1H), 7.48 (t, J=7 Hz 2H), 7.4 (t, J=7 Hz, 1H).

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-4d04a666af86495ea0bedbba01129a5b
出典データセット
uspto-grants-2009_12
特許番号
US07635695B2

反応ノート

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