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Ethanol hydrochloride → HCID 178479177, 화합물

HRID 1409401
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HRID 1409401 반응식
Cl.CCO.[Cl:5][C:6]1[CH:13]=[C:12]([C:14]2[N:18](C3CCCCO3)[N:17]=[CH:16][CH:15]=2)[CH:11]=[CH:10][C:7]=1[C:8]#[N:9]>>[ClH:5].[Cl:5][C:6]1[CH:13]=[C:12]([C:14]2[CH:15]=[CH:16][NH:17][N:18]=2)[CH:11]=[CH:10][C:7]=1[C:8]#[N:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21887872Ethanol hydrochlorideHCID 706562532-chloro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)benzonitrile

생성물 1

HCID 178479177HCID 178479177, 화합물수율 166.6%

반응 조건

온도
10 °C

실험 절차

HCl/EtOH ˜10% (35.1 ml, 115 mmol) was set into the reaction flask under nitrogen atmosphere. 2-Chloro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-benzonitrile (12 g, 46.2 mmol) was added. The mixture was cooled to 10° C. and agitated for 2 h. Temperature was set to 0° C. and the mixture was stirred additional 2 hours. The precipitation was filtered, washed with ethanol and dried under vacuum overnight to obtain 9.24 g of the title compound. 1H-NMR (400 MHz, DMSO-d6): δ 6.99 (d, 3H), 7.86 (d, 1H), 7.96-8.02 (m, 2H), 8.14-8.17 (m, 1H).

후처리

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
  1. customwas set to 0° C.
  2. stirringthe mixture was stirred additional 2 hours
  3. customThe precipitation
  4. filtrationwas filtered
  5. washwashed with ethanol
  6. customdried under vacuum overnight

출처 및 근거

ORD 기록
ord-104115c1ffd948fa995b9d8138415759
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921378B2

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