Benzyl Bromide → HCID 20059716、化合物

HRID 1085551ノート

反応式

HRID 1085551 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([CH2:9][C:10]([OH:12])=[O:11])=[C:4]([CH3:13])[CH:3]=1.[H-].[Na+].[CH2:16](Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>CN(C)C=O>[CH2:16]([O:1][C:2]1[CH:3]=[C:4]([CH3:13])[C:5]([CH2:9][C:10]([O:12][CH2:13][C:4]2[CH:5]=[CH:6][CH:7]=[CH:2][CH:3]=2)=[O:11])=[C:6]([CH3:8])[CH:7]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 126604274-Hydroxy-2,6-dimethylbenzeneacetic acid

生成物 1

HCID 20059716HCID 20059716、化合物収率 161.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.36 g of 2-(4-hydroxy-2,6-dimethylphenyl)acetic acid was treated with 184 mg of a 60% dispersion of sodium hydride in mineral oil and 0.72 g of benzyl bromide in 10 ml of dry dimethylformamide. The solvent was removed by evaporation and the residue was partitioned between water and methylene chloride. The organic layer was evaporated to give 0.63 g of crude product of melting point 54°-57° C. Recrystallization from aqueous methanol gave 0.58 g of pure benzyl 2-(4-benzyloxy-2.6-dimethylphenyl)acetate of melting point 62°-64° C.

後処理

  1. customThe solvent was removed by evaporation
  2. customthe residue was partitioned between water and methylene chloride
  3. customThe organic layer was evaporated
  4. customto give 0.63 g of crude product of melting point 54°-57° C
  5. customRecrystallization from aqueous methanol

出典と根拠

ORDレコード
ord-b2af7a42e55841c9a65aff3f57137c49
出典データセット
uspto-grants-1991_04
特許番号
US05010060

反応ノート

読み込み中…