Trifluoroacetic acid → 3-(1H-pyrazol-4-yl)-pyridine-2,6-diamine

HRID 77877ノート

反応式

HRID 77877 の反応式
C([N:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[CH:29][CH:30]=2)[CH:22]=[N:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[CH:29][CH:30]=2)[CH:22]=[N:21]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59255416HCID 59255416、化合物

生成物 1

HCID 592551723-(1H-pyrazol-4-yl)-pyridine-2,6-diamine収率 60%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-(1-trityl-1H-pyrazol-4-yl)-pyridin-2,6-diamine (10.0 g, 25.7 mmol) described in Manufacturing Example 36-1-1 in methylene chloride (14 mL) was added trifluoroacetic acid (7 mL) under nitrogen atmosphere, which was stirred for 1 hour at room temperature. The reaction mixture was concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate, then ethyl acetate:methanol=10:1) to obtain the title compound (600 mg, 60%).

後処理

  1. concentrationThe reaction mixture was concentrated under a reduced pressure
  2. customThe residue was purified by NH silica gel column chromatography (ethyl acetate

出典と根拠

ORDレコード
ord-6ef575f901f14b698e170b2b33a948ff
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

反応ノート

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