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Water → HCID 178473748、化合物

HRID 1061696
ノート
印刷プレビュー

反応式

HRID 1061696 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].[Cl-].[Al+3].[Cl-].[Cl-].C(OC([C@@H](N[C:25]([CH2:27][N:28]1[C:33]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[CH:32][N:31]([C:40](=O)[CH3:41])[CH:30]([CH:43]([CH3:45])[CH3:44])[C:29]1=[O:46])=O)CC1C=CC=CC=1)C#N)(=O)C.[OH2:47]>O1CCCC1>[C:40]([N:31]1[CH:32]=[C:33]([C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)[N:28]([C@@H:27]([CH2:25][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:29]([C:30]2[NH:31][N:3]=[N:2][N:1]=2)[OH:46])[C:29](=[O:46])[CH:30]1[CH:43]([CH3:45])[CH3:44])(=[O:47])[CH3:41]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 60073844(2RS,3S)-2-Acetoxy-3-{(3RS)-4-acetyl-3-isopropyl-2-oxo-6-phenyl-1,2,3,4-tetrahydropyrazin-1-yl}methylcarbonylamino-4-phenylbutanenitrile

生成物 1

HCID 178473748HCID 178473748、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
60 °C

実験手順

Sodium azide (75.3 mg) and aluminum chloride (386 mg) are added to a solution of (2RS,3S)-2-acetoxy-3-{(3RS)-4-acetyl-3-isopropyl-2-oxo-6-phenyl-1,2,3,4-tetrahydropyrazin-1-yl}methylcarbonylamino-4-phenylbutanenitrile (299 mg, Compound No. 18-1) in tetrahydrofuran (3.5 ml), and the mixture is stirred for two hours. The reaction mixture is warmed to 60° C. and stirred for three hours. The reaction mixture is cooled to room temperature, then water is added to the reaction mixture, and the whole is extracted with ethyl acetate. The extract is washed with saturated brine and dried over anhydrous magnesium sulfate. The extract is concentrated under reduced pressure, and the resulting residue is purified by silica gel column chromatography to give the titled compound (242 mg).

後処理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. extractionthe whole is extracted with ethyl acetate
  3. washThe extract is washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationThe extract is concentrated under reduced pressure
  6. customthe resulting residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c8aa1168fb8f41f78427b08467f8e8f5
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06960575B2

反応ノート

読み込み中…

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