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Sodium Hydroxide → HCID 68912635、化合物

HRID 732629
ノート
印刷プレビュー

反応式

HRID 732629 の反応式
[C:1]([O:5][C:6]([N:8]([CH2:21][C@@H:22]1[C@@H:26]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:25][N:24]([C:33](=[O:42])[CH2:34][CH2:35][CH2:36][CH2:37][C:38]([O:40]C)=[O:39])[CH2:23]1)[C@@H:9]([C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1)[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>CO>[C:1]([O:5][C:6]([N:8]([CH2:21][C@@H:22]1[C@@H:26]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH2:25][N:24]([C:33](=[O:42])[CH2:34][CH2:35][CH2:36][CH2:37][C:38]([OH:40])=[O:39])[CH2:23]1)[C@@H:9]([C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1)[CH3:10])=[O:7])([CH3:2])([CH3:3])[CH3:4]
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 14798Sodium HydroxideHCID 68913838HCID 68913838、化合物

生成物 1

HCID 68912635HCID 68912635、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 270 mg portion of methyl 6-[(3R,4S)-3-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-4-phenylpyrrolidin-1-yl]-6-oxohexanoate was dissolved in 3 ml of methanol, mixed with 3 ml of 1 M sodium hydroxide aqueous solution and stirred at room temperature for 4Hours. The reaction solution was concentrated under a reduced pressure, and 1 M hydrochloric acid was added to the residue until it became pH 3.0. After extraction with chloroform and subsequent washing with saturated brine, the organic layer was dried with anhydrous sodium sulfate and concentrated under a reduced pressure. The thus obtained residue was purified by a silica gel column chromatography (chloroform-methanol) to obtain 237 mg of 6-[(3R,4S)-3-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-4-phenylpyrrolidin-1-yl]-6-oxohexanoic acid as a colorless solid. FP: 559.

後処理

  1. concentrationThe reaction solution was concentrated under a reduced pressure, and 1 M hydrochloric acid
  2. additionwas added to the residue until it
  3. extractionAfter extraction with chloroform
  4. washsubsequent washing with saturated brine
  5. dry with materialthe organic layer was dried with anhydrous sodium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customThe thus obtained residue was purified by a silica gel column chromatography (chloroform-methanol)

出典と根拠

ORDレコード
ord-6170f573da334406a20e3040fa9a8e67
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07585886B2

反応ノート

読み込み中…

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