Ammonia → HCID 68626960, 화합물

HRID 1886965노트

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HRID 1886965 반응식
Br[CH:2]1[C:8]2=[N:9][C:10]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][N:15]=3)=[CH:11][C:12](=[O:13])[N:7]2[CH2:6][CH2:5][O:4][CH2:3]1.[NH3:20]>>[NH2:20][CH:2]1[C:8]2=[N:9][C:10]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][N:15]=3)=[CH:11][C:12](=[O:13])[N:7]2[CH2:6][CH2:5][O:4][CH2:3]1

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 68626997(+/-)-9-Bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4-a-diaza-benzocyclohepten-4-one

생성물 1

HCID 68626960HCID 68626960, 화합물수율 44%

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온도
100 °C

실험 절차

A suspension of 18.7 g (57.89 mmol) of (+/−)-9-bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4-a-diaza-benzocyclohepten-4-one in 520 mL of ammonia (7N solution in MeOH) in sealed tubes was stirred at 100° C. for 4 hours. The cooled solution was evaporated to remove solvent. After an acido-basic work-up and extraction with dichloromethane, the mixture was washed with saturated solution of sodium chloride. The organic phase was dried over sodium sulfate and concentrated. The residue was organised in diethyl ether to afford 6.70 g (44%) of product as a yellow solid.

후처리

  1. customThe cooled solution was evaporated
  2. customto remove solvent
  3. extractionAfter an acido-basic work-up and extraction with dichloromethane
  4. washthe mixture was washed with saturated solution of sodium chloride
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c247c14fc20c440aaf2dac6287cabd3d
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501728B2

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