Water → {1-[4-(4-Fluoro-phenyl)phthalazin-1-yl]piperidin-4-yl}-methyl-carbamic acid tert-butyl ester

HRID 1012961

반응식

HRID 1012961 반응식
[C:1]([O:5][C:6](=[O:15])[N:7]([CH3:14])[CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].Cl[C:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:20]([C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=2)=[N:19][N:18]=1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[C:1]([O:5][C:6](=[O:15])[N:7]([CH:8]1[CH2:13][CH2:12][N:11]([C:17]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[C:20]([C:27]3[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=3)=[N:19][N:18]=2)[CH2:10][CH2:9]1)[CH3:14])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 21152391-Chloro-4-(4-fluorophenyl)phthalazineHCID 27568064-N-Boc-4-N-Methyl-aminopiperidine

생성물 1

HCID 58157128{1-[4-(4-Fluoro-phenyl)phthalazin-1-yl]piperidin-4-yl}-methyl-carbamic acid tert-butyl ester수율 95.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Combine methyl-piperidin-4-yl-carbamic acid tert-butyl ester (75 g, 349 mmol), 1-chloro-4-(4-fluoro-phenyl)-phthalazine (75 g, 289 mmol), and potassium carbonate (80 g, 579 mmol) in dimethyl sulfoxide (500 mL) and heat the mixture to 110° C. for 3 h. Cool the reaction to ambient temperature and pour the slurry into water (1.0 L). Collect the solids by filtration and dry in a vacuum oven for 3 days to provide the title compound as a white solid (120 g, 95%). ES/MS m/z 437.3 (M+1).

후처리

  1. temperatureCool
  2. customthe reaction to ambient temperature
  3. customCollect the solids
  4. filtrationby filtration
  5. customdry in a vacuum oven for 3 days

출처 및 근거

ORD 기록
ord-52d5ae3a476f4396aa21aac3175b0b4d
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981892B2

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