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Hydrogen chloride-ethyl acetate → HCID 178479653, 화합물

HRID 1620773
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HRID 1620773 반응식
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:27]=[CH:26][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH2:20][CH2:21][O:22][CH2:23][CH2:24][OH:25])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:8][CH2:7]1.[ClH:36].C(OCC)(=O)C>COC(C)(C)C>[ClH:36].[F:35][C:2]([F:1])([F:34])[C:3]1[CH:29]=[C:28]([C:30]([F:32])([F:33])[F:31])[CH:27]=[CH:26][C:4]=1[CH2:5][N:6]1[CH2:7][CH2:8][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH2:20][CH2:21][O:22][CH2:23][CH2:24][OH:25])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:10][CH2:11]1
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참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 178518154HCID 178518154, 화합물

생성물 1

HCID 178479653HCID 178479653, 화합물

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매

실험 절차

To a solution of (5Z)-5-({1-[2,4-bis(trifluoromethyl)benzyl]piperidin-4-yl}methylidene)-4-{[2-(2-hydroxyethoxy)ethyl]amino}-1,3-thiazol-2(5H)-one (7.86 g) in tert-butyl methyl ether (70 mL) was added dropwise a solution of 4N hydrogen chloride/ethyl acetate (3.74 mL), and the mixture was stirred at room temperature for 1 hr. The precipitate was collected by filtration, and the obtained solid was recrystallized from ethanol/heptane to give the title compound (5.63 g).

후처리

  1. filtrationThe precipitate was collected by filtration
  2. customthe obtained solid was recrystallized from ethanol/heptane

출처 및 근거

ORD 기록
ord-0e796c9c4aff404982063d1fb65028f1
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772277B2

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