Acetone → 3-(3'-Chloro-2'-hydroxypropyl)-benzhydrol

HRID 1731173노트

반응식

HRID 1731173 반응식
[Cl:1][CH2:2][C:3](=[O:19])[CH2:4][C:5]1[CH:6]=[C:7]([C:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:8]=[CH:9][CH:10]=1.CC([O-])C.CC([O-])C.CC([O-])C.[Al+3].CC(C)=O>C(O)(C)C>[Cl:1][CH2:2][CH:3]([OH:19])[CH2:4][C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][CH:10]=1)[CH:11]([OH:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 11143Aluminum isopropoxideHCID 214956283'(3'-Chloro-2'-oxo-propyl)-benzophenone

생성물 1

HCID 214956193-(3'-Chloro-2'-hydroxypropyl)-benzhydrol수율 105%

시약·촉매·용매 1

HCID 3776Isopropanol용매4회

반응 조건

온도
50 °C

실험 절차

A solution of 11.23 g of 3'(3'-chloro-2'-oxo-propyl)-benzophenone in 112 ml of isopropanol was added to 50 ml of isopropanol and 17 g of aluminum isopropylate heated to 50° C and the mixture was refluxed for 2 hours while slowly distilling isopropanol and the acetone formed while keeping the volume constant by adding 30 ml of isopropanol. The mixture was concentrated to 50 ml and after returning to room temperature, the mixture was added with stirring to a mixture of ice-water-hydrochloride acide. The mixture was extracted with methylene chloride and the organic phase was washed with water, dried over sodium sulfate, treated with activated carbon, filtered and evaporated to dryness to obtain 11.97 g of 3-(3'-chloro-2'-hydroxypropyl)-benzhydrol which was used as is for the next step.

후처리

  1. concentrationThe mixture was concentrated to 50 ml
  2. customafter returning to room temperature
  3. additionthe mixture was added
  4. extractionThe mixture was extracted with methylene chloride
  5. washthe organic phase was washed with water
  6. dry with materialdried over sodium sulfate
  7. additiontreated with activated carbon
  8. filtrationfiltered
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0d631c1af48e434fa4a58c42195a4d40
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03995056

반응 노트

불러오는 중…