Hydrogen Bromide → (+/-)-9-Amino-2-pyrimidin-4-yl-6,7,8,9-tetrahydro-5H-1,4a,7-triaza-benzocyclohepten-4-one dihydrobromide

HRID 1890415노트

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HRID 1890415 반응식
C(OC([N:6]1[CH2:12][CH:11]([NH2:13])[C:10]2=[N:14][C:15]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][N:20]=3)=[CH:16][C:17](=[O:18])[N:9]2[CH2:8][CH2:7]1)=O)C.[BrH:25]>C(O)(=O)C>[BrH:25].[BrH:25].[NH2:13][CH:11]1[C:10]2=[N:14][C:15]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][N:20]=3)=[CH:16][C:17](=[O:18])[N:9]2[CH2:8][CH2:7][NH:6][CH2:12]1

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 669298339-amino-4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4-a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester

생성물 1

HCID 68731596(+/-)-9-Amino-2-pyrimidin-4-yl-6,7,8,9-tetrahydro-5H-1,4a,7-triaza-benzocyclohepten-4-one dihydrobromide수율 125.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

To a solution of 9.70 g (23.59 mmol) of (+/−)-9-amino-4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester dissolved in 118 mL of glacial acetic acid was added 41.38 mL (235.86 mmol) of hydrobromic acid (33 wt % solution in glacial acetic acid). The resulting mixture was stirred at 90° C. for 16 hours, cooled and evaporated to dryness. Toluene was added to the residue and evaporated. Ethanol was added to the residue and evaporated. The crude was triturated with diethyl ether and filtered to afford 12.40 g of the product as a brown powder.

후처리

  1. temperaturecooled
  2. customevaporated to dryness
  3. additionToluene was added to the residue
  4. customevaporated
  5. additionEthanol was added to the residue
  6. customevaporated
  7. customThe crude was triturated with diethyl ether
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-9e1a75f481ce47938732572a86a2f51c
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507476B2

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