Hydrochloric Acid → 1,2,3,4-Tetrahydro-isoquinoline-7-carboxylic acid (4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-yl)-amide hydrochloride

HRID 1886967ノート

反応式

HRID 1886967 の反応式
C(OC([N:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([C:18](=[O:38])[NH:19][CH:20]3[C:26]4=[N:27][C:28]([C:32]5[CH:37]=[CH:36][N:35]=[CH:34][N:33]=5)=[CH:29][C:30](=[O:31])[N:25]4[CH2:24][CH2:23][O:22][CH2:21]3)=[CH:13][CH:14]=2)[CH2:9]1)=O)(C)(C)C.[ClH:39]>ClCCl>[ClH:39].[O:31]=[C:30]1[N:25]2[C:26]([CH:20]([NH:19][C:18]([C:12]3[CH:11]=[C:10]4[C:15]([CH2:16][CH2:17][NH:8][CH2:9]4)=[CH:14][CH:13]=3)=[O:38])[CH2:21][O:22][CH2:23][CH2:24]2)=[N:27][C:28]([C:32]2[CH:37]=[CH:36][N:35]=[CH:34][N:33]=2)=[CH:29]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 44159737HCID 44159737、化合物

生成物 1

HCID 866498491,2,3,4-Tetrahydro-isoquinoline-7-carboxylic acid (4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-yl)-amide hydrochloride収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.049 g (0.10 mmol) of (+/−)-7-(4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-ylcarbamoyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (example 1) dissolved in 0.5 mL of dichloromethane was added 0.24 mL (0.96 mmol) of hydrochloric acid (4M in dioxane). The resulting mixture was stirred at room temperature for 2.5 hours. The resulting residue was filtered, washed with dichloromethane and isopropylether to afford 0.031 g (70%) of the pure product as a yellow powder.

後処理

  1. filtrationThe resulting residue was filtered
  2. washwashed with dichloromethane and isopropylether

出典と根拠

ORDレコード
ord-54a47bbc66724967a22e644acfdf4d13
出典データセット
uspto-grants-2013_08
特許番号
US08501728B2

反応ノート

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