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

HRID 385399ノート

反応式

HRID 385399 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c1582c16a555434ba277451c80134e2e
出典データセット
uspto-grants-2013_02
特許番号
US08367863B2

反応ノート

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