Phosphorus sulfide (P2S5) → HCID 86676949、化合物

HRID 710092ノート

反応式

HRID 710092 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([S:16]([CH3:19])(=[O:18])=[O:17])=[CH:12][C:11]=2[F:20])=[C:4]([F:22])[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:24]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[S:24])[C:10]2[CH:15]=[CH:14][C:13]([S:16]([CH3:19])(=[O:18])=[O:17])=[CH:12][C:11]=2[F:20])=[C:4]([F:22])[CH:3]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 71257495HCID 71257495、化合物

生成物 1

HCID 86676949HCID 86676949、化合物収率 48.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Intermediate 32 (1 g, 2.56 mmol) dissolved in toluene (10 ml) and added P2S5 (0.57 g, 2.56 mmol). This mixture was refluxed for 18 h. Toluene removed on rotavapour to obtain the crude. Crude was purified by column chromatography on 60-120 mesh silicagel using EtOAc and Petether (20:80) as eluent to afford the title compound (500 mg) as a yellow solid. 1H-NMR (δ ppm, DMSO-d6, 400 MHz): 11.02 (s, 1H), 7.92-7.85 (m, 2H), 7.69 (dd, J 1.6, 8.1, 1H), 7.63 (dd, J 1.6, 9, 1H), 7.33-7.27 (m, 2H), 3.02 (s, 3H).

後処理

  1. temperatureThis mixture was refluxed for 18 h
  2. customToluene removed on rotavapour
  3. customto obtain the crude
  4. customCrude was purified by column chromatography on 60-120 mesh silicagel

出典と根拠

ORDレコード
ord-389dddae9f2c4311a3ccbf96a094982d
出典データセット
uspto-grants-2015_11
特許番号
US09181214B2

反応ノート

読み込み中…