Sodium Hydroxide → cis-1-Benzyl-2-oxo-5-phenyl-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-propionic acid

HRID 1419037노트

반응식

HRID 1419037 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][C:13]3[CH:18]=[CH:17][C:16](OC)=[CH:15][C:14]=3OC)[C:10](=[O:23])[C@@H:9](CC(O)=O)[O:8][C@H:7]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3Cl)[C:6]=2[CH:35]=1.[OH-:36].[Na+]>CO.Cl>[CH2:12]([N:11]1[C:5]2[CH:4]=[CH:3][CH:2]=[CH:35][C:6]=2[C@H:7]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[O:8][C@H:9]([CH2:5][CH2:6][C:7]([OH:8])=[O:36])[C:10]1=[O:23])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 69946224trans-7-Chloro-5-(2-chlorophenyl)-1-(2,4-dimethoxybenzyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

생성물 1

HCID 69945752cis-1-Benzyl-2-oxo-5-phenyl-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-propionic acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

In 20 ml of methanol was dissolved 0.5 g of ethyl ester of cis-1-benzyl-2-oxo-5-phenyl-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-propionic acid obtained in Example 8. To the solution was added 7 ml of 1N sodium hydroxide, and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was acidified with 100 ml of IN hydrochloric acid, which was subjected to extraction with 150 ml of ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate. Then the solvent was distilled off under reduced pressure to leave 0.46 g of cis-1-benzyl-2-oxo-5-phenyl-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-propionic acid as plates, m.p. 112°-114° C.

후처리

  1. extractionwas subjected to extraction with 150 ml of ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThen the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-3feb133eda864b71842bf5d3055dd530
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05885979

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