Hydrochloric Acid → 5-Benzyloxy-2-[(4-benzyloxy-phenyl)-(4-fluoro-phenylamino)-methyl]-5-(4-fluoro-phenyl)-pentanoic acid methyl ester

HRID 1052896

반응식

HRID 1052896 반응식
[CH2:1]([O:8][CH:9]([C:50]1[CH:55]=[CH:54][C:53]([F:56])=[CH:52][CH:51]=1)[CH2:10][CH2:11][CH:12]([CH:27]([C:36]1[CH:41]=[CH:40][C:39]([O:42][CH2:43][C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)=[CH:38][CH:37]=1)[NH:28][C:29]1[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=1)C(N1C(C2C=CC=CC=2)COC1=O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O-].[Na+].[CH3:60][O:61][C:62](=O)[O:63]C.Cl>ClCCl>[CH3:60][O:61][C:62](=[O:63])[CH:12]([CH:27]([C:36]1[CH:37]=[CH:38][C:39]([O:42][CH2:43][C:44]2[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=2)=[CH:40][CH:41]=1)[NH:28][C:29]1[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=1)[CH2:11][CH2:10][CH:9]([O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:50]1[CH:55]=[CH:54][C:53]([F:56])=[CH:52][CH:51]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 12021Dimethyl CarbonateHCID 10942334Sodium MethoxideHCID 667135533-[5-Benzyloxy-2-[(4-benzyloxy-phenyl)-(4-fluoro-phenylamino)-methyl]-5-(4-fluoro-phenyl)-pentanoyl]-4-phenyl-oxazolidin-2-one

생성물 1

HCID 667134205-Benzyloxy-2-[(4-benzyloxy-phenyl)-(4-fluoro-phenylamino)-methyl]-5-(4-fluoro-phenyl)-pentanoic acid methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

10 gms of 3-[5-Benzyloxy-2-[(4-benzyloxy-phenyl)-(4-fluoro-phenylamino)-methyl]-5-(4-fluoro-phenyl)-pentanoyl]-4-phenyl-oxazolidin-2-one was taken in dichloromethane, to this 3.6 gms of sodium methoxide was added followed by 3.2 ml of dimethylcarbonate, and 500 ml of dichloromethane. Reaction mass was stirred for about 5-7 hours. To the reaction mass 0.1 ml of hydrochloric acid was added. Separated the layers and extract the aqueous layer with 25 ml of methylene dichloride. The organic layer was washed with water and dried over sodium sulphate. Distilled the solvent completely under reduced pressure at 50-55° C. and 85 ml of methanol was added. Stirred the reaction mass for about 1-2 hours, filtered and washed with methanol and dried at 50-55° C. to get 5 gms of 5-Benzyloxy-2-[(4-benzyloxy-phenyl)-(4-fluoro-phenylamino)-methyl]-5-(4-fluoro-phenyl)-pentanoic acid methyl ester.

후처리

  1. additionwas added
  2. customReaction mass
  3. customSeparated the layers
  4. extractionextract the aqueous layer with 25 ml of methylene dichloride
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulphate
  7. distillationDistilled the solvent completely under reduced pressure at 50-55° C.
  8. addition85 ml of methanol was added
  9. stirringStirred the reaction mass for about 1-2 hours
  10. filtrationfiltered
  11. washwashed with methanol
  12. customdried at 50-55° C.

출처 및 근거

ORD 기록
ord-e4a6f5330f9e4afa9ff377e872d238b3
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388440B2

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