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

HRID 639622
ノート
印刷プレビュー

反応式

HRID 639622 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 887Methanol溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d161a2bd9dbf416985b73b798edd4693
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691877B2

反応ノート

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