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Water → HCID 22013867、化合物

HRID 1532740
ノート
印刷プレビュー

反応式

HRID 1532740 の反応式
[H-].[Na+].[H][H].C1(C)C=CC(S([O:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[O:20][C:21]=2[CH3:22])(=O)=O)=CC=1.[OH2:30].[C:31]([O:34][CH2:35][CH3:36])(=[O:33])[CH3:32]>CCCCCC.CN(C)C=O>[C:17]([NH:18][CH:32]([CH2:19][C:23]1[CH:28]=[CH:27][C:26]([O:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[O:20][C:21]=2[CH3:22])=[CH:25][CH:24]=1)[C:31]([O:34][CH2:35][CH3:36])=[O:33])(=[O:30])[CH3:16]
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

8

反応物 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 120517392-(5-Methyl-2-phenyloxazol-4-yl)ethyl 4-methylbenzenesulfonateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22013867HCID 22013867、化合物収率 37%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回
HCID 8058Hexane溶媒

反応条件

温度
80 °C

実験手順

Sodium hydride (60% in oil, 440 mg, 11.0 mmol) was washed twice with n-hexane (5 ml) under a nitrogen atmosphere, and suspended in N,N-dimethylformamide (50 ml) and ice-cooled. To this suspension was added ethyl N-acetyl-L-tyrosine ester (2.51 g, 10.0 mmol) over 15 min. Ten minutes later when hydrogen bubbling ended, a solution of 2-(5-methyl-2-phenyl-4-oxazolyl)ethyl p-toluenesulfonate (3.57 g, 10.0 mmol) in N,N-dimethylformamide (50 ml) was added. The mixture was stirred at 80° C. for 3 hr, and water (50 ml) and ethyl acetate (100 ml×2) were added for partition. The obtained organic layer was washed with saturated brine (100 ml), dried over magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (developing solvent; dichloromethane:methanol=98:2) to give the title compound (1.63 g, yield 37%) as a white solid.

後処理

  1. temperatureice-cooled
  2. customfor partition
  3. washThe obtained organic layer was washed with saturated brine (100 ml)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (developing solvent; dichloromethane:methanol=98:2)

出典と根拠

ORDレコード
ord-ab95d491c880408ab9b1fc146f1b27d2
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06204277B1

反応ノート

読み込み中…

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