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Triethylamine → 5-Amino-1-(4-fluorophenyl)-N-(3,3,3-trifluoro-2-{[(2-fluoroethyl)amino]methyl}-2-hydroxypropyl)-1H-pyrazole-4-carboxamide

HRID 886716
ノート
印刷プレビュー

反応式

HRID 886716 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([NH:16][CH2:17][C:18]1([C:21]([F:24])([F:23])[F:22])[CH2:20][O:19]1)=[O:15].Cl.[F:26][CH2:27][CH2:28][NH2:29].C(N(CC)CC)C>C(#N)C>[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([NH:16][CH2:17][C:18]([CH2:20][NH:29][CH2:28][CH2:27][F:26])([OH:19])[C:21]([F:23])([F:22])[F:24])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9995Ethanamine, 2-fluoro-, hydrochlorideHCID 594874985-amino-1-(4-fluorophenyl)-N-{[2-(trifluoromethyl)-2-oxiranyl]methyl}-1H-pyrazole-4-carboxamide

生成物 1

HCID 591872345-Amino-1-(4-fluorophenyl)-N-(3,3,3-trifluoro-2-{[(2-fluoroethyl)amino]methyl}-2-hydroxypropyl)-1H-pyrazole-4-carboxamide収率 128.5%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

To a solution of 5-amino-1-(4-fluorophenyl)-N-{[2-(trifluoromethyl)-2-oxiranyl]methyl}-1H-pyrazole-4-carboxamide (1.03 g, 3 mmol) in anhydrous acetonitrile (10 ml) was added 2-fluoroethylamine hydrochloride (650 mg, 6 mmol, ca. 90% purity) and triethylamine (0.98 ml, 7 mmol) and the resulting suspension was shaken for 4 days. It was partitioned between ethyl acetate (70 ml) and water (20 ml), washed with saturated brine (20 ml), dried over sodium sulphate and evaporated to give a gum (1.57 g). This was purified on 100 g SiO2 using the Flashmaster 2 with 0-100°/0 ethyl acetate in cyclohexane 60 minute gradient as eluent. This gave the title compound (924 mg).

後処理

  1. customIt was partitioned between ethyl acetate (70 ml) and water (20 ml)
  2. washwashed with saturated brine (20 ml)
  3. dry with materialdried over sodium sulphate
  4. customevaporated

出典と根拠

ORDレコード
ord-38358a0a626447e284a8d81171153a8f
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08247377B2

反応ノート

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