Lithium Hydroxide → HCID 22876405, 화합물

HRID 1377167노트

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HRID 1377167 반응식
[C:1]([NH:8][C@H:9]([C@H:17]1[O:21][C:20](=[O:22])[C@H:19]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]3[O:30][CH2:31][O:32][C:26]=3[CH:25]=2)[CH2:18]1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=O.[OH-:33].[Li+].C[O:36]CCOC>O.C(OCC)(=O)C.C1COCC1>[C:1]([NH:8][C@@H:9]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C@@H:17]([OH:21])[CH2:18][C@@H:19]([CH2:23][C:24]1[CH:29]=[CH:28][C:27]2[O:30][CH2:31][O:32][C:26]=2[CH:25]=1)[C:20]([OH:22])=[O:36])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:33]

참가 물질

7

반응물 3

HCID 3939Lithium HydroxideHCID 80711,2-DimethoxyethaneHCID 70149639HCID 70149639, 화합물

생성물 1

HCID 22876405HCID 22876405, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 278 mg of 5(S)-[1(S)-(Boc-amino)-2-phenylethyl]-3(R)-[(3,4-methylenedioxyphenyl)methyl]dihydrofuran-2-(3H)-one in 10.25 ml of ethylene glycol dimethyl ether and 5.15 ml of water is treated dropwise, at RT, with 2,53 ml of a 1M lithium hydroxide solution. After that, the reaction mixture is stirred at RT for 3 h, diluted with ethyl acetate and THF, and washed in a separating funnel until neutral with a mixture consisting of 31 ml of sat. ammonium chloride solution and 2.6 ml of 10% citric acid solution, followed by saline and water. The title compound, which is subjected to further processing without any further purification, is obtained after drying over sodium sulfate and removing the solvent. FAB-MS (M+H)+ =458.

후처리

  1. washwashed in a separating funnel until neutral with a mixture
  2. customThe title compound, which is subjected to further processing without any further purification
  3. customis obtained
  4. dry with materialafter drying over sodium sulfate
  5. customremoving the solvent

출처 및 근거

ORD 기록
ord-cee874ba6d514a128360db2974483ef1
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663200

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