Sodium hydride → N-(2-isopropyloxyethyl)isatic acid anhydride

HRID 1975370

반응식

HRID 1975370 반응식
[C:1]1([C:8]([C:10]([O:12][C:13](=[O:23])[C:14](=[O:22])[C:15]2[C:16](=[CH:18][CH:19]=[CH:20][CH:21]=2)[NH2:17])=[O:11])=[O:9])[C:2](=[CH:4][CH:5]=[CH:6][CH:7]=1)[NH2:3].[H-].[Na+].S(C1C=CC(C)=CC=1)(O[CH2:30][CH2:31][O:32][CH:33]([CH3:35])[CH3:34])(=O)=O>O=P(N(C)C)(N(C)C)N(C)C>[CH:33]([O:32][CH2:31][CH2:30][NH:3][C:2]1[C:1]([C:8]([C:10]([O:12][C:13](=[O:23])[C:14](=[O:22])[C:15]2[C:16](=[CH:18][CH:19]=[CH:20][CH:21]=2)[NH:17][CH2:30][CH2:31][O:32][CH:33]([CH3:34])[CH3:35])=[O:11])=[O:9])=[CH:7][CH:6]=[CH:5][CH:4]=1)([CH3:35])[CH3:34]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 12914357IsatinsaureanhydridHCID 190994432-Isopropoxyethyl 4-methylbenzenesulfonate

생성물 1

HCID 53681304N-(2-isopropyloxyethyl)isatic acid anhydride

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매2회

실험 절차

The starting material is prepared as follows: 3 g of isatic acid anhydride are dissolved in 50 ml of distilled hexametapol(=hexamethylphosphoric acid triamide). The solution is cooled to 5°, and 0.96 g of 55% NaH (freed of oil with hexane) is added. The mixture is stirred for 30 minutes at RT and then 5.67 g of O-(2-isopropyloxyethyl) tosylate are added. The mixture is stirred for 30 minutes at RT and for one hour at 50°. The mixture is left to stand overnight and is poured onto ice, and the organic layer is separated off and washed with water. The mixture is concentrated by evaporation, and the residue is digested with ether and filtered off with suction, yielding N-(2-isopropyloxyethyl)isatic acid anhydride, m.p. 107°-108°.

후처리

  1. customThe starting material is prepared
  2. temperatureThe solution is cooled to 5°
  3. stirringThe mixture is stirred for 30 minutes at RT and for one hour at 50°
  4. waitThe mixture is left
  5. waitto stand overnight
  6. additionis poured onto ice
  7. customthe organic layer is separated off
  8. washwashed with water
  9. concentrationThe mixture is concentrated by evaporation
  10. filtrationfiltered off with suction

출처 및 근거

ORD 기록
ord-9bd2642b51de4fb08f43035628853c24
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286728

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