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Succinic anhydride → HCID 67088928、化合物

HRID 1910378
ノート
印刷プレビュー

反応式

HRID 1910378 の反応式
[CH3:1][C:2]1([CH3:26])[C:10]2([O:15][C:14]3[CH:16]=[CH:17][C:18]([N+:20]([O-:22])=[O:21])=[CH:19][C:13]=3[CH:12]=[CH:11]2)[N:9]([CH2:23][CH2:24][OH:25])[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.C(N(CC)CC)C.[C:34]1(=[O:40])[O:39][C:37](=[O:38])[CH2:36][CH2:35]1>CN(C)C1C=CN=CC=1.ClCCl>[CH3:1][C:2]1([CH3:26])[C:3]2[C:8](=[CH:7][CH:6]=[CH:5][CH:4]=2)[N:9]([CH2:23][CH2:24][O:25][C:34](=[O:40])[CH2:35][CH2:36][C:37]([OH:39])=[O:38])[C:10]21[CH:11]=[CH:12][C:13]1[C:14](=[CH:16][CH:17]=[C:18]([N+:20]([O-:22])=[O:21])[CH:19]=1)[O:15]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7922Succinic anhydrideHCID 8471TriethylamineHCID 31048582-(3',3'-Dimethyl-6-nitrospiro[1-benzopyran-2,2'-indol]-1'(3'H)-yl)ethan-1-ol

生成物 1

HCID 67088928HCID 67088928、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane
溶媒

実験手順

About 2 g of 1-(2-Hydroxyethyl)-3,3-dimethylindolino-6′-nitrobenzopyrylospiran (TCI America), about 0.44 ml of triethylamine, and about 0.69 g of 4-(dimethylamino)pyridine were dissolved in about 30 ml of dichloromethane. After addition of about 0.59 g of succinic anhydride, the solution was stirred under Ar at room temperature for about 19 hours. The mixture was washed with 5% aqueous hydrochloric acid, aqueous sodium bicarbonate, and water, then dried over magnesium sulfate. After the solvent was distilled off, the concentrated solution was added dropwise to hexane under stirring. The resulting solid was collected by filtration to yield 4-(2-(3′,3′-dimethyl-6-nitrospiro[chromene-2,2′-indoline]-1′-yl)ethoxy)-4-oxobutanoic acid.

後処理

  1. washThe mixture was washed with 5% aqueous hydrochloric acid, aqueous sodium bicarbonate, and water
  2. dry with materialdried over magnesium sulfate
  3. distillationAfter the solvent was distilled off
  4. additionthe concentrated solution was added dropwise to hexane
  5. stirringunder stirring
  6. filtrationThe resulting solid was collected by filtration

出典と根拠

ORDレコード
ord-00e6d514360346e691e004786f7658fe
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08603944B2

反応ノート

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