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

HRID 1890400ノート

反応式

HRID 1890400 の反応式
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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

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 (step 1.4) 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.

後処理

  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

出典と根拠

ORDレコード
ord-632c5309b1a741eba52eb6ca86f4ec7d
出典データセット
uspto-grants-2013_08
特許番号
US08507475B2

反応ノート

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