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Succinic anhydride → HCID 67088928, 화합물

HRID 1910378
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HRID 1910378 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 67088928HCID 67088928, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344
Dichloromethane
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00e6d514360346e691e004786f7658fe
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08603944B2

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