Sodium Hydroxide → HCID 12133110、化合物

HRID 1581527ノート

反応式

HRID 1581527 の反応式
[O:1]([C:8]1[N:13]=[C:12]([C:14](Cl)=[O:15])[CH:11]=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][C:25]([N:27]2[CH2:31][CH:30]([N:32]3[CH2:37][CH2:36][O:35][CH2:34][CH2:33]3)[CH2:29][NH:28]2)=[O:26])=[CH:20][CH:19]=1.[OH-].[Na+]>C(Cl)Cl.O.C(Cl)Cl>[F:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][C:25]([N:27]2[CH2:31][CH:30]([N:32]3[CH2:37][CH2:36][O:35][CH2:34][CH2:33]3)[CH2:29][N:28]2[C:14]([C:12]2[CH:11]=[CH:10][N:9]=[C:8]([O:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[N:13]=2)=[O:15])=[O:26])=[CH:20][CH:19]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 129701582-Phenoxypyrimidine-4-carbonyl chlorideHCID 219922062-(4-Fluorophenyl)-1-(4-morpholin-4-yl-pyrazolidin-1-yl)ethanone

生成物 1

HCID 12133110HCID 12133110、化合物収率 23%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21908982Water methylene chloride溶媒2 回

実験手順

2-Phenoxypyrimidine-4-carbonyl chloride, 18, (0.07 g, 0.28 mmol) in methylene chloride (1.5 mL) is added dropwise to a suspension of 2-(4-fluorophenyl)-1-(4-morpholin-4-yl-pyrazolidin-1-yl)ethanone, 13, (0.06 g, 0.18 mmol) in a 2:5 water/CH2Cl2 solution (7 mL) containing NaOH (0.0112 g, 0.28 mmol) at room temperature. The solution is stirred 18 hours and diluted with additional 2:5 water/CH2Cl2. The layers are allowed to separate and the aqueous phase extracted with additional methylene chloride. The organic layers are combined, dried, filtered and concentrated in vacuo to afford a tan solid which is purified by preparative HPLC to provide 0.021 g (23% yield) of the desired product as an oily solid.

後処理

  1. customto separate
  2. extractionthe aqueous phase extracted with additional methylene chloride
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto afford a tan solid which
  7. customis purified by preparative HPLC

出典と根拠

ORDレコード
ord-af66ff4b2e50489face03c7ae6a9bb2a
出典データセット
uspto-grants-2004_05
特許番号
US06730668B2

反応ノート

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