Methanol → trans-5-(4-Ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

HRID 1419067

반응식

HRID 1419067 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C@@H:10]2[C:16]3[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=3[N:14]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[C:13](=[O:27])[C@@H:12]([CH2:28][C:29]([O:31]CC)=[O:30])[O:11]2)=[C:6]([O:34][CH3:35])[CH:5]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].CO.O1CCCC1>O>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C@@H:10]2[C:16]3[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=3[N:14]([CH2:22][C:23]([CH3:25])([CH3:26])[CH3:24])[C:13](=[O:27])[C@@H:12]([CH2:28][C:29]([OH:31])=[O:30])[O:11]2)=[C:6]([O:34][CH3:35])[CH:5]=1)[CH3:2]

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 67603127Ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

생성물 1

HCID 10140397trans-5-(4-Ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (0.18 g), potassium carbonate (0.10 g), methanol (10 ml), tetrahydrofuran (10 ml) and water (5 ml) was refluxed for 1.5 h. The resulting mixture was concentrated in vacuo, acidified with 1N hydrochloric acid (50 ml) and extracted with ethyl acetate (50 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo to give trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid as colorless crystals (mp=230°-232° C.).

후처리

  1. temperaturewas refluxed for 1.5 h
  2. concentrationThe resulting mixture was concentrated in vacuo
  3. extractionextracted with ethyl acetate (50 ml)
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-69a7df2ea17847a7a38817f76b847774
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05885979

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