Thionyl Chloride → HCID 4935532, 화합물

HRID 2278158

반응식

HRID 2278158 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:10]2[CH:15]=[CH:14][C:13](Br)=[CH:12][CH:11]=2)O)=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[C:21]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]>C(Cl)Cl>[C:21]([N:28]1[CH2:29][CH2:30][N:31]([CH:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5]2[CH:6]=[CH:7][CH:2]=[CH:3][CH:4]=2)[CH2:32][CH2:33]1)([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]

참가 물질

5

반응물 3

HCID 24386Thionyl ChlorideHCID 143452tert-Butyl piperazine-1-carboxylateHCID 5204294,4'-Dibromobenzhydrol

생성물 1

HCID 4935532HCID 4935532, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirring solution of bis(4-bromophenyl)methanol (0.060 mmol) in CH2Cl2 (0.3 mL) was added thionyl chloride (40 μL, 0.60 mmol) and the reaction mixture was stirred for 48 h. The reaction was evaporated to dryness under a stream of N2 and the crude product redissolved in acetonitrile (1.0 mL). 1-Boc-piperazine (22.3 mg, 0.12 mmol) was added and the reaction mixture was refluxed for 4 h. The reaction mixture was concentrated under reduced pressure, redissolved in CH2Cl2 and passed through a short pad of SiO2, providing the 1-Boc-4-diphenylmethylpiperazine.

후처리

  1. customThe reaction was evaporated to dryness under a stream of N2
  2. dissolutionthe crude product redissolved in acetonitrile (1.0 mL)
  3. temperaturethe reaction mixture was refluxed for 4 h
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionredissolved in CH2Cl2

출처 및 근거

ORD 기록
ord-ba3e0929aa8e462081f04aea86fa36ba
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133148B2

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