2-Chloroethanol → 1-[Bis(4-fluorophenyl)methoxy]-2-chloroethane

HRID 35296

반응식

HRID 35296 반응식
[Cl:1][CH2:2][CH2:3][OH:4].S(=O)(=O)(O)O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)O)=[CH:13][CH:12]=1.O>C1C=CC=CC=1>[Cl:1][CH2:2][CH2:3][O:4][CH:17]([C:14]1[CH:15]=[CH:16][C:11]([F:10])=[CH:12][CH:13]=1)[C:19]1[CH:20]=[CH:21][C:22]([F:25])=[CH:23][CH:24]=1

참가 물질

6

반응물 4

HCID 342-ChloroethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 1230494,4'-Difluorobenzhydryl alcohol

생성물 1

HCID 107793021-[Bis(4-fluorophenyl)methoxy]-2-chloroethane

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

A mixture of 20 parts of 2-chloroethanol, 3 parts of sulfuric acid and 16 parts of benzene was heated on a water-bath. Then there were added dropwise 35 parts of 4-fluoro-α-(4-fluorophenyl)benzenemethanol dissolved in 32 parts of benzene. After the addition was complete, the whole was stirred and refluxed for 4 hours. After cooling the reaction mixture was poured into water. The benzene layer was separated, dried over calcium chloride and evaporated. The residue was distilled in vacuo, yielding 35 parts of 1,1'-[(2-chloroethoxy)methylene]bis[4-fluorobenzene]; bp. 164°-166° C. at 1.5 mm. pressure; nD20 : 1.5462; d2020 : 1.2290 (intermediate 1).

후처리

  1. temperaturewas heated on a water-bath
  2. additionAfter the addition
  3. temperaturerefluxed for 4 hours
  4. temperatureAfter cooling the reaction mixture
  5. customThe benzene layer was separated
  6. dry with materialdried over calcium chloride
  7. customevaporated
  8. distillationThe residue was distilled in vacuo

출처 및 근거

ORD 기록
ord-aa649f34fbe0408682aae1bc3a34ceb5
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766125

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