Dibah → (2-Chloro-4-methylphenyl)methanol

HRID 420754

반응식

HRID 420754 반응식
[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].CC(C[Al]CC(C)C)C>ClCCl>[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=1[CH2:4][OH:5]

참가 물질

4

반응물 2

HCID 16682954DibahHCID 22019481Methyl 2-chloro-4-methylbenzoate

생성물 1

HCID 15544016(2-Chloro-4-methylphenyl)methanol수율 82.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methyl 2-chloro-4-methylbenzoate (520 mg, 2.82 mmol) was dissolved in Dichloromethane (DCM) (15 mL) and at 0° C. Dibal-H (4.694 ml, 7.04 mmol) was slowly added. The mixture was left at 0° C. for 2H and then at room temperature overnight. Next morning HPLC showed no starting material remaining, reaction was quenched with Rochelle salt, and leaving under stirring for 1 hour and then it was extracted with DCM, dried and concentrated to afford 365 mg of the final compound, pure enough to be used in the next step.

후처리

  1. waitThe mixture was left at 0° C. for 2H
  2. customat room temperature
  3. customovernight
  4. customreaction
  5. customwas quenched with Rochelle salt
  6. customleaving
  7. extractionit was extracted with DCM
  8. customdried
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d8e7fb9e4deb49f58b3479ebbf6b83e1
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097628B2

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