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HCID 14479916, 화합물 → HCID 178469348, 화합물

HRID 1762983
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HRID 1762983 반응식
[CH3:1][C:2]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:10]2[C:5](=[CH:6][C:7]([NH:14][C:15]([C:17]3[CH:22]=[N:21][CH:20]=[CH:19][N:18]=3)=O)=[C:8]([N+:11]([O-])=O)[CH:9]=2)[NH:4][C:3]1=[O:23]>[Pd].C(O)C>[CH3:1][C:2]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:10]2[C:5](=[CH:6][C:7]3[NH:14][C:15]([C:17]4[CH:22]=[N:21][CH:20]=[CH:19][N:18]=4)=[N:11][C:8]=3[CH:9]=2)[NH:4][C:3]1=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 14479916HCID 14479916, 화합물

생성물 1

HCID 178469348HCID 178469348, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매2회

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온도
60 °C

실험 절차

3.2 g. (8.3 mmol) 3-methyl-3-ethoxycarbonyl-5-nitro-6-(2-pyrazinoylamino)-indolin-2-one in 100 ml. ethanol are hydrogenated in 100 ml. ethanol in the presence of 0.5 g. 10% palladium on charcoal. After completion of the take up of hydrogen, the solution is filtered off from the catalyst, the ethanol is evaporated off and the residue is stirred for 1 hour in glacial acetic acid at 60° C. The glacial acetic acid is evaporated, the residue is taken up in water, filtered and recrystallized from ethanol. There are obtained 1.8 g (65% of theory) of the title compound, m.p. 288°-290° C.

후처리

  1. filtrationAfter completion of the take up of hydrogen, the solution is filtered off from the catalyst
  2. customthe ethanol is evaporated off
  3. customThe glacial acetic acid is evaporated
  4. filtrationfiltered
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-c687f0adcae04df2bd9f91fe7d37e1cd
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04835280

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