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Thionyl Chloride → 4-[3-(4-Tert-butylaminocarbonylphenyl)-3-chloroprop-1-yl]-1-tritylimidazole

HRID 478003
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반응식

HRID 478003 반응식
[C:1]([NH:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH:14](O)[CH2:15][CH2:16][C:17]2[N:18]=[CH:19][N:20]([C:22]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:21]=2)=[CH:10][CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].S(Cl)([Cl:44])=O>C(Cl)Cl>[C:1]([NH:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH:14]([Cl:44])[CH2:15][CH2:16][C:17]2[N:18]=[CH:19][N:20]([C:22]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:21]=2)=[CH:10][CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 140972094-[3-(4-Tert-butylaminocarbonylphenyl)-3-hydroxyprop-1-yl]-1-tritylimidazole

생성물 1

HCID 140972104-[3-(4-Tert-butylaminocarbonylphenyl)-3-chloroprop-1-yl]-1-tritylimidazole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 3.21 g of 4-[3-(4-tert-butylaminocarbonylphenyl)-3-hydroxyprop-1-yl]-1-tritylimidazole and 1.5 ml of thionyl chloride in 50 ml of methylene chloride is refluxed for 1 h, cooled and poured into 50 ml of ice-cold sodium bicarbonate solution. The organic phase is separated, dried over sodium sulfate and evaporated to yield 4-[3-(4-tert-butylaminocarbonylphenyl)-3-chloroprop-1-yl]-1-tritylimidazole as a white foam. NMR (CDCl3): δ=1.45 (s,9H), 4.30 (t,J=6.0 Hz, 2H).

후처리

  1. temperaturecooled
  2. customThe organic phase is separated
  3. dry with materialdried over sodium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-39da7d435cd14b55808b48a7c30f1f16
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889861

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