Sodium Hydroxide → HCID 12133110, 화합물

HRID 1061613노트

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HRID 1061613 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 12133110HCID 12133110, 화합물수율 23%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 21908982Water methylene chloride용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3e3df849b87b4485bb561ac600e0303b
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960593B2

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