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 1890404노트

반응식

HRID 1890404 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 44159005HCID 44159005, 화합물

생성물 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 ester수율 1,186.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2abe86c3552d424dafa1ef63fbac1e65
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507475B2

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