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Water → N2,N4-Dibenzyl-6-trifluoromethyl-pyridine-2,3,4-triamine

HRID 639622
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HRID 639622 반응식
[CH2:1]([NH:8][C:9]1[C:14]([N+:15]([O-])=O)=[C:13]([NH:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:12]=[C:11]([C:26]([F:29])([F:28])[F:27])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O>C1COCC1.CO.[Ni]>[CH2:1]([NH:8][C:9]1[C:14]([NH2:15])=[C:13]([NH:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:12]=[C:11]([C:26]([F:29])([F:28])[F:27])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 962WaterHCID 67453795N2,N4-Dibenzyl-3-nitro-6-trifluoromethyl-pyridine-2,4-diamine

생성물 1

HCID 67456850N2,N4-Dibenzyl-6-trifluoromethyl-pyridine-2,3,4-triamine수율 68%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 887Methanol용매2회
HCID 8028
Tetrahydrofuran
용매

실험 절차

N2,N4-Dibenzyl-3-nitro-6-trifluoromethyl-pyridine-2,4-diamine (15.9 g, 35.6 mmol) was dissolved in a mixture of THF (100 ml) and MeOH (200 ml). Raney Nickel (3.18 g, 20 wt %) was added and the mixture was stirred at room temperature under 80 psi H2 for 1 hour. The mixture was filtered through celite to remove the catalyst and the filtrate was concentrated in vacuo to give an oil. Trituration in MeOH with a small amount of water gave a precipitate which was collected by filtration, washed with cold MeOH and dried in vacuo to give the title compound (9.02 g) as a white solid.

후처리

  1. filtrationThe mixture was filtered through celite
  2. customto remove the catalyst
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto give an oil
  5. filtrationwas collected by filtration
  6. washwashed with cold MeOH
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-d161a2bd9dbf416985b73b798edd4693
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691877B2

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