Triethylamine → (2-Chloro-4-methylphenyl)methyl acetate

HRID 420755

反応式

HRID 420755 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[CH2:9][OH:10].CCN(CC)CC.[C:18](OCl)([CH3:20])=[O:19]>ClCCl.O>[C:18]([O:10][CH2:9][C:3]1[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[Cl:1])(=[O:19])[CH3:20]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 12616564Chloro methylformateHCID 15544016(2-Chloro-4-methylphenyl)methanol

生成物 1

HCID 58001748(2-Chloro-4-methylphenyl)methyl acetate収率 97.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of (2-chloro-4-methylphenyl)methanol (365 mg, 2.331 mmol) and Et3N (0.390 mL, 2.80 mmol) in Dichloromethane (DCM) (10 mL) at 0° C. AcOCl (0.331 mL, 4.66 mmol) was slowly added and the mixture was left under stirring at 0° C. for 1 hour then at room temperature overnight. Next morning HPLC showed no starting material remaining volatiles were removed under vacuum and resulting crude was dissolved in DCM washed several times with water. Organic layers were dried over Na2SO4 and volatiles removed to afford 453 mg of the final compound as a brown oil.

後処理

  1. customat 0° C
  2. waitthe mixture was left
  3. customat room temperature
  4. customovernight
  5. customwere removed under vacuum
  6. customresulting crude
  7. dry with materialOrganic layers were dried over Na2SO4 and volatiles
  8. customremoved

出典と根拠

ORDレコード
ord-257647a2e19c492eab35db16d4826c57
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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