Lithium Hydroxide → HCID 22876405、化合物

HRID 1377167ノート

反応式

HRID 1377167 の反応式
[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]

参加物

7

反応物 3

HCID 3939Lithium HydroxideHCID 80711,2-DimethoxyethaneHCID 70149639HCID 70149639、化合物

生成物 1

HCID 22876405HCID 22876405、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cee874ba6d514a128360db2974483ef1
出典データセット
uspto-grants-1997_09
特許番号
US05663200

反応ノート

読み込み中…