Ethanol hydrochloride → Ethyl 2-(3-(cyclopropylmethoxy)-4-nitrophenyl)acetate

HRID 1183666노트

반응식

HRID 1183666 반응식
[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH2:15][C:16]([OH:18])=[O:17])[CH:9]=[CH:10][C:11]=2[N+:12]([O-:14])=[O:13])[CH2:3][CH2:2]1.[CH2:19](O)[CH3:20].Cl>>[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:9]=[CH:10][C:11]=2[N+:12]([O-:14])=[O:13])[CH2:2][CH2:3]1

참가 물질

3

반응물 2

HCID 21887872Ethanol hydrochlorideHCID 579955402-(3-(Cyclopropylmethoxy)-4-nitrophenyl)acetic acid

생성물 1

HCID 57995474Ethyl 2-(3-(cyclopropylmethoxy)-4-nitrophenyl)acetate

실험 절차

2-(3-(cyclopropylmethoxy)-4-nitrophenyl)acetic acid (40 g, 143 mmol) was dissolved in 20% EtOH—HCl solution (200 ml) and refluxed for 3 h to convert the starting material to ester. The volatiles were removed under reduced pressure and the residue was extracted with ethyl acetate (×2). The combined organic extracts were washed with water, dried (Na2SO4), filtered and concentrated under reduced pressure. The crude material was purified by re crystallization to ethyl 2-(3-(cyclopropylmethoxy)-4-nitrophenyl)acetate (38 g) as pale yellow solid.

후처리

  1. temperaturerefluxed for 3 h
  2. customThe volatiles were removed under reduced pressure
  3. extractionthe residue was extracted with ethyl acetate (×2)
  4. washThe combined organic extracts were washed with water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe crude material was purified by re crystallization to ethyl 2-(3-(cyclopropylmethoxy)-4-nitrophenyl)acetate (38 g) as pale yellow solid

출처 및 근거

ORD 기록
ord-8f10c755f1f94d5abe82e713977c7008
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664249B2

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