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Ethanol → HCID 22239012, 화합물

HRID 1743358
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HRID 1743358 반응식
[CH2:1]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([CH2:17][CH2:18][CH2:19][C:20]#[N:21])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN.[CH2:25](O)[CH3:26]>[Ni]>[CH2:25]([NH:21][CH2:20][CH2:19][CH2:18][CH2:17][C:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[N:9]=1)[CH3:26]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 222390171-Benzyl-3-(3-cyanopropyl)indazole

생성물 1

HCID 22239012HCID 22239012, 화합물수율 26%

시약·촉매·용매 1

HCID 935Nickel촉매

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온도
70 °C

실험 절차

A solution of 1-benzyl-3-(3-cyanopropyl)indazole (100 mg, 0.35 mM) in ethanol (10 ml) was stirred at room temperature and Raney nickel (approx. 100 mg, wet weight) was added. The resulting suspension was warned to 65° C. and hydrazine hydrate (0.1 ml, 87 mg) added carefully. The mixture was stirred at 70° C. for a further 2 hr then cooled and filtered through celite. Solvent was removed in vacuo and the residue purified by chromatography on silica (chloroform/methanol 9:1) to give the title product as a clear oil (25 mg, 26%).

후처리

  1. customwas warned to 65° C.
  2. temperaturethen cooled
  3. filtrationfiltered through celite
  4. customSolvent was removed in vacuo
  5. customthe residue purified by chromatography on silica (chloroform/methanol 9:1)

출처 및 근거

ORD 기록
ord-0e29daf820b2474094b4dcef7348b42c
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07009056B2

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