Neopentyl glycol → HCID 15407351, 화합물

HRID 571225노트

반응식

HRID 571225 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][C:8](=[O:13])[C:7]2=[O:14])([O-:3])=[O:2].[CH3:15][C:16]([CH3:21])([CH2:19]O)[CH2:17][OH:18].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1CCCCC1>[CH3:15][C:16]1([CH3:21])[CH2:17][O:18][C:7]2([C:6]3[C:10](=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=3)[NH:9][C:8]2=[O:13])[O:14][CH2:19]1

참가 물질

5

반응물 3

HCID 31344Neopentyl glycolHCID 521998p-Toluenesulfonic acid monohydrateHCID 46692505-Nitroisatin

생성물 1

HCID 15407351HCID 15407351, 화합물수율 108.9%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

A mixture of 5-nitroindoline-2,3-dione (305 mg, 1.587 mmol), 2,2-dimethylpropane-1,3-diol (165 mg, 1.587 mmol) and p-toluenesulfonic acid monohydrate (catalytic amount) in cyclohexane (9 ml) was stirred at reflux temperature (removing water by a Dean-Stark apparatus) for 6 hours. The reaction was cooled to room temperature and the solid was recovered by filtration and washed with petroleum ether, affording 5,5-dimethyl-5′-nitrospiro[[1,3]dioxane-2,3′-indolin]-2′-one (481 mg). that was used as such in the following step. MS/ESI+ 279.0 [MH]+.

후처리

  1. temperatureat reflux temperature (
  2. customremoving water by a Dean-Stark apparatus) for 6 hours
  3. filtrationthe solid was recovered by filtration
  4. washwashed with petroleum ether

출처 및 근거

ORD 기록
ord-ee582f49e5684a7091a1c6097a3cfc06
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09024027B2

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