Ammonia → HCID 68626960、化合物

HRID 1890239ノート

反応式

HRID 1890239 の反応式
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

参加物

3

反応物 2

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

生成物 1

HCID 68626960HCID 68626960、化合物収率 44%

反応条件

温度
100 °C

実験手順

A suspension of 18.7 g (57.89 mmol) of (+/−)-9-bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4a-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.

後処理

  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

出典と根拠

ORDレコード
ord-dccb9c530f154c7c8322ad6f741de69f
出典データセット
uspto-grants-2013_08
特許番号
US08507470B2

反応ノート

読み込み中…