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

HRID 420754

反応式

HRID 420754 の反応式
[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]

参加物

4

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8e7fb9e4deb49f58b3479ebbf6b83e1
出典データセット
uspto-grants-2012_01
特許番号
US08097628B2

関連ノート

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