Hydrochloric Acid → (+/-)-4-Oxo-2-pyridin-4-yl-9-[(1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester

HRID 1890404ノート

反応式

HRID 1890404 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:12][CH:11]([NH:13][C:14]([C:16]2[CH:25]=[C:24]3[C:19]([CH2:20][CH2:21][N:22](C(OC(C)(C)C)=O)[CH2:23]3)=[CH:18][CH:17]=2)=[O:15])[C:10]2=[N:33][C:34]([C:38]3[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=3)=[CH:35][C:36](=[O:37])[N:9]2[CH2:8][CH2:7]1)=[O:5])[CH3:2].Cl>ClCCl>[CH2:1]([O:3][C:4]([N:6]1[CH2:12][CH:11]([NH:13][C:14]([C:16]2[CH:25]=[C:24]3[C:19]([CH2:20][CH2:21][NH:22][CH2:23]3)=[CH:18][CH:17]=2)=[O:15])[C:10]2=[N:33][C:34]([C:38]3[CH:39]=[CH:40][N:41]=[CH:42][CH:43]=3)=[CH:35][C:36](=[O:37])[N:9]2[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 44159005HCID 44159005、化合物

生成物 1

HCID 44159256(+/-)-4-Oxo-2-pyridin-4-yl-9-[(1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester収率 1,186.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.0265 g (0. mmol) of (+/−)-9-[(2-tert-butoxycarbonyl-1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-4-oxo-2-pyridin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester (example 5) dissolved in 1 mL of dichloromethane was added 1.13 mL (4.50 mmol) of hydrochloric acid (4M in dioxane). The resulting mixture was stirred at room temperature for 16 hours. The resulting residue was filtered, washed with dichloromethane and isopropylether to afford 0.261 g (100%) of the pure product as a white 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-2abe86c3552d424dafa1ef63fbac1e65
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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