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

HRID 420755

반응식

HRID 420755 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-257647a2e19c492eab35db16d4826c57
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097628B2

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