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Trifluoroacetic acid → HCID 22462762, 화합물

HRID 1937174
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인쇄 미리보기

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HRID 1937174 반응식
Cl.Cl.[N:3]1([CH2:8][CH2:9][O:10][C:11]2[CH:40]=[CH:39][C:14]([CH2:15][C:16]3[C:17]4[CH:38]=[CH:37][CH:36]=[CH:35][C:18]=4[S:19][C:20]=3[C:21]3[CH:26]=[CH:25][C:24]([NH:27][C:28]([C:30]4N=CN[CH:34]=4)=[O:29])=[CH:23][CH:22]=3)=[CH:13][CH:12]=2)[CH2:7][CH2:6][CH2:5][CH2:4]1.C(C1C[CH2:47][C:46](=[O:49])[CH2:45]1)(O)=O.[NH4+].[OH-].[C:52]([C:56]([OH:58])=[O:57])([F:55])([F:54])[F:53]>C(Cl)(Cl)Cl.CO>[F:53][C:52]([F:55])([F:54])[C:56]([OH:58])=[O:57].[N:3]1([CH2:8][CH2:9][O:10][C:11]2[CH:40]=[CH:39][C:14]([CH2:15][C:16]3[C:17]4[CH:38]=[CH:37][CH:36]=[CH:35][C:18]=4[S:19][C:20]=3[C:21]3[CH:22]=[CH:23][C:24]([NH:27][C:28]([CH:30]4[CH2:34][CH2:47][C:46](=[O:49])[CH2:45]4)=[O:29])=[CH:25][CH:26]=3)=[CH:13][CH:12]=2)[CH2:4][CH2:5][CH2:6][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 14923Ammonium HydroxideHCID 2277983-Oxocyclopentanecarboxylic acidHCID 178478890HCID 178478890, 화합물

생성물 1

HCID 22462762HCID 22462762, 화합물수율 98%

시약·촉매·용매 2

HCID 887Methanol
용매
2회
HCID 6212Chloroform용매

실험 절차

By essentially following the conditions described in Example 1, Part F, the free base of the title compound was prepared as a foam from 2-(4-aminophenyl)-3-[4-[2-(1-pyrrolidinyl)ethoxy]benzyl]benzo[b]thiophene (Example 16; Part D) and 3-carboxycyclopentanone in 98% yield following radial chromatography (SiO2; 1% then 2% then 5% MeOH in CHCl3 sat'd with NH4OH). The solid was taken up in 5 mL of MeOH and was treated with 1.2 eq of CF3CO2H. The solution was concentrated in vacuo to give the title compound.

후처리

  1. concentrationThe solution was concentrated in vacuo
  2. customto give the title compound

출처 및 근거

ORD 기록
ord-5b6089006ea644bdb5965417cb1cf09f
출처 데이터셋
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06391901B1

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