Thionyl Chloride → HCID 4935532、化合物

HRID 2278158

反応式

HRID 2278158 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 4935532HCID 4935532、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ba3e0929aa8e462081f04aea86fa36ba
出典データセット
uspto-grants-2015_09
特許番号
US09133148B2

関連ノート

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