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Dichloromethane → HCID 178485780, 화합물

HRID 24853
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인쇄 미리보기

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HRID 24853 반응식
C1(=O)[N:5]([CH2:6][C:7]([N:9]([C:11]2[CH:16]=[CH:15][C:14]([NH:17]/[C:18](=[C:25]3\[C:26](=[O:37])[NH:27][C:28]4[C:33]\3=[CH:32][C:31]([N+:34]([O-:36])=[O:35])=[CH:30][CH:29]=4)/[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:13][CH:12]=2)[CH3:10])=[O:8])C(=O)C2=CC=CC=C12.ClCCl.O.NN>C(O)C>[NH2:5][CH2:6][C:7]([N:9]([C:11]1[CH:16]=[CH:15][C:14]([NH:17]/[C:18](=[C:25]2\[C:26](=[O:37])[NH:27][C:28]3[C:33]\2=[CH:32][C:31]([N+:34]([O-:36])=[O:35])=[CH:30][CH:29]=3)/[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[CH:13][CH:12]=1)[CH3:10])=[O:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 178485775HCID 178485775, 화합물

생성물 1

HCID 178485780HCID 178485780, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

287 mg (0.5 mmol) of (Z)-3-{1-[4-(N-phthalimidomethylcarbonyl-N-methylamino)phenylamino]-1-phenyl-methylidene}-5-nitro-2-indolinone are suspended in 20 ml of ethanol and 20 ml of dichloromethane and after the addition of 0.3 ml of 80% hydrazine hydrate solution stirred for 18 hours at 50° C. The mixture is then cooled to ambient temperature, the insoluble matter is suction filtered and the mother liquor is concentrated by evaporation. The residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=92:8:0.8) and the product is again triturated with methanol, suction filtered and dried.

후처리

  1. temperatureThe mixture is then cooled to ambient temperature
  2. filtrationfiltered
  3. concentrationthe mother liquor is concentrated by evaporation
  4. customThe residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=92:8:0.8)
  5. customthe product is again triturated with methanol, suction
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-2b5a4c8ab2a3437a9bdb9357e75d0e10
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06855710B2

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