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ethyl (2R,3R)-3-{[(2S)-4-methyl-1-oxo-1-{4-[(2,3,4-trimethoxyphenyl)methyl]piperazin-1-yl}pentan-2-yl]carbamoyl}oxirane-2-carboxylate → HCID 23700901、化合物

HRID 1982503
ノート
印刷プレビュー

反応式

HRID 1982503 の反応式
[OH-].[Na+:2].C(O)C.[CH3:6][CH:7]([CH3:42])[CH2:8][C@H:9]([NH:31][C:32]([C@@H:34]1[O:36][C@H:35]1[C:37]([O:39]CC)=[O:38])=[O:33])[C:10]([N:12]1[CH2:17][CH2:16][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=2[O:29][CH3:30])[CH2:14][CH2:13]1)=[O:11]>C(O)C>[CH3:6][CH:7]([CH3:42])[CH2:8][C@H:9]([NH:31][C:32]([C@@H:34]1[O:36][C@H:35]1[C:37]([O-:39])=[O:38])=[O:33])[C:10]([N:12]1[CH2:13][CH2:14][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=2[O:29][CH3:30])[CH2:16][CH2:17]1)=[O:11].[Na+:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6917749ethyl (2R,3R)-3-{[(2S)-4-methyl-1-oxo-1-{4-[(2,3,4-trimethoxyphenyl)methyl]piperazin-1-yl}pentan-2-yl]carbamoyl}oxirane-2-carboxylateHCID 23692425Sodium hydroxide ethanol

生成物 1

HCID 23700901HCID 23700901、化合物収率 98%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Under cooling with ice, a 0.48N sodium hydroxide-ethanol solution (9.48 ml) was added to an ethanol solution (20 ml) of ethyl trans-3-[(s)-3-methyl-1-{4-(2,3,4-trimethoxyphenylmethyl)piperazine-1-yl carbonyl}butylcarbamoyl]-oxirane-2-carboxylate (2.38 g) obtained above, and the mixture was stirred at room temperature for 2.5 hours. After removal of ethanol by distillation under reduced pressure, water was added, and any insoluble matters were removed by filtration using sellaite. The filtrate was concentrated and dried under reduced pressure to yield 2.31 g of sodium trans-3-[(s)-3-methyl-1-{4-(2,3,4-trimethoxyphenylmethyl)piperazine-1-yl carbonyl}butylcarbamoyl]oxirane-2-carboxylate as a light yellow powder (yield: 98%).

後処理

  1. temperatureUnder cooling with ice
  2. customobtained above, and the mixture
  3. customAfter removal of ethanol
  4. distillationby distillation under reduced pressure, water
  5. additionwas added
  6. customany insoluble matters were removed by filtration
  7. concentrationThe filtrate was concentrated
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6ad4ab21b0094001a3aa9d4576c6fd20
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04596803

反応ノート

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