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4-Methylmorpholine → HCID 178445898、化合物

HRID 1607411
ノート
印刷プレビュー

反応式

HRID 1607411 の反応式
[CH2:1]([CH:8]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:9]([OH:11])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.[NH2:31][C@H:32]([C:39]([NH:41][C@H:42]([CH:47]=[N:48][NH:49][C:50]([NH2:52])=[O:51])[CH2:43][CH:44]([CH3:46])[CH3:45])=[O:40])[CH2:33][C:34]1[N:38]=[CH:37][NH:36][CH:35]=1.CN1CCOCC1>CN(C)C=O.ClCCl>[CH2:12]([CH:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:9]([NH:31][C@H:32]([C:39]([NH:41][C@H:42]([CH:47]=[N:48][NH:49][C:50]([NH2:52])=[O:51])[CH2:43][CH:44]([CH3:46])[CH3:45])=[O:40])[CH2:33][C:34]1[N:38]=[CH:37][NH:36][CH:35]=1)=[O:11])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 64800Benzenepropanoic acid, alpha-(phenylmethyl)-HCID 682631,1'-CarbonyldiimidazoleHCID 178445905HCID 178445905、化合物

生成物 1

HCID 178445898HCID 178445898、化合物収率 30.5%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

A mixture of 240 mg of 2-benzyl-3-phenylpropionic acid and 170 mg of 1,1'-carbonyldiimidazole was added to 10 ml of dry dichloromethane, and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was added to a solution of 650 mg of L-histidyl-L-leucinal semicarbazone.2p-toluenesulfonic acid salt and 200 mg of N-methylmorpholine in 10 ml of dry N,N-dimethylformamide, and the mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, and a 5% aqueous sodium bicarbonate solution was added to the residue. The mixture was extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel flash column chromatography (eluent: dichloromethane/methanol=10/1 by volume) to obtain 162 mg of N-(2-benzyl-3-phenylpropionyl)-L-histidyl-L-leucinal semicarbazone as a white powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiona 5% aqueous sodium bicarbonate solution was added to the residue
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel flash column chromatography (eluent: dichloromethane/methanol=10/1 by volume)

出典と根拠

ORDレコード
ord-bd30c918bb404affa131e936175b07fe
出典データセット
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04863904

反応ノート

読み込み中…

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