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Thionyl Chloride → HCID 18955940, 화합물

HRID 2379687
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반응식

HRID 2379687 반응식
[Br:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH:4](O)[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1.S(Cl)([Cl:19])=O>ClCCl>[Br:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH:4]([Cl:19])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 12319462HCID 12319462, 화합물

생성물 1

HCID 18955940HCID 18955940, 화합물수율 76%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The crude benzhydryl alcohol from above (31.8 g, 107 mmole) was dissolved in 150 ml of dichloromethane and 11.7 ml (1.5 equiv.) of thionyl chloride was added dropwise over ten minutes. The solution was stirred overnight at room temperature and the solvent was removed under vacuum. The crude product was redissolved in 100 ml of toluene and the solvent was again removed under vacuum in order to eliminate excess thionyl chloride, providing crude product as a dark oil. The material was purified by short path distillation (Kugelrohr apparatus, 150° C., 0.5 mm) to give 25.8 g (76%) of (2-bromophenyl)chloro(4-chlorophenyl)methane as a pale yellow oil.

후처리

  1. customthe solvent was removed under vacuum
  2. dissolutionThe crude product was redissolved in 100 ml of toluene
  3. customthe solvent was again removed under vacuum in order
  4. customproviding crude product as a dark oil
  5. distillationThe material was purified by short path distillation (Kugelrohr apparatus, 150° C., 0.5 mm)

출처 및 근거

ORD 기록
ord-bc45a6fe05094f3cae132e383b144839
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364843

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