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Bromine → (S)-(+)-5-Bromo-2-(2-methylbutyloxy)benzonitrile

HRID 442585
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반응식

HRID 442585 반응식
[CH3:1][C@@H:2]([CH2:13][CH3:14])[CH2:3][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[C:7]#[N:8].[Br:15]Br>C(Cl)(Cl)Cl>[Br:15][C:10]1[CH:11]=[CH:12][C:5]([O:4][CH2:3][C@@H:2]([CH3:1])[CH2:13][CH3:14])=[C:6]([CH:9]=1)[C:7]#[N:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408Bromine2회HCID 53752700(S)-(+)-2-(2-Methylbutyloxy)benzonitrile

생성물 1

HCID 53787839(S)-(+)-5-Bromo-2-(2-methylbutyloxy)benzonitrile

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of compound 39 (4.25 g, 0.022 mol), bromine (12.31 g, 0.077 mol) and chloroform (50 ml) was heated under reflux overnight. A further portion of bromine (12.31 g, 0.077 mol) was then added and heating continued for another 24 h. The resultant solution was washed with a saturated solution of sodium thiosulphate and finally with water. The dichloromethane solution was dried (MgSO4) and evaporated in vacuo and the crude oil was purified by column chromatography (10% petrol/dichloromethane) to yield a fawn oil.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. temperatureheating
  4. washThe resultant solution was washed with a saturated solution of sodium thiosulphate and finally with water
  5. dry with materialThe dichloromethane solution was dried (MgSO4)
  6. customevaporated in vacuo
  7. customthe crude oil was purified by column chromatography (10% petrol/dichloromethane)
  8. customto yield a fawn oil

출처 및 근거

ORD 기록
ord-e1ca72e799b648e0995c63b172e3a78d
출처 데이터셋
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05891358

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