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1,5-Dimethyl-1H-pyrazol-4-amine dihydrochloride → (3R)-1-(2-((1,5-dimethyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile

HRID 714871
ノート
印刷プレビュー

反応式

HRID 714871 の反応式
Cl[C:2]1[N:7]=[C:6]([N:8]2[CH2:12][CH2:11][C@:10]([CH2:15][CH3:16])([C:13]#[N:14])[C:9]2=[O:17])[CH:5]=[CH:4][N:3]=1.Cl.Cl.[CH3:20][N:21]1[C:25]([CH3:26])=[C:24]([NH2:27])[CH:23]=[N:22]1>CC(O)C>[CH3:20][N:21]1[C:25]([CH3:26])=[C:24]([NH:27][C:2]2[N:7]=[C:6]([N:8]3[CH2:12][CH2:11][C@:10]([CH2:15][CH3:16])([C:13]#[N:14])[C:9]3=[O:17])[CH:5]=[CH:4][N:3]=2)[CH:23]=[N:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 446309061,5-Dimethyl-1H-pyrazol-4-amine dihydrochlorideHCID 117840665(3R)-1-(2-chloropyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile

生成物 1

HCID 117840341(3R)-1-(2-((1,5-dimethyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile収率 69.7%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A solution of (3R)-1-(2-chloropyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile (100 mg) obtained in Step A of Example 8 and 1,5-dimethyl-1H-pyrazol-4-amine dihydrochloride (73 mg) in propan-2-ol (4.0 mL) was stirred in a microwave reactor at 160° C. for 1 hr, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate), and recrystallized (diisopropyl ether/ethyl acetate) to give the title compound (90 mg).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. customThe obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate)
  3. customrecrystallized (diisopropyl ether/ethyl acetate)

出典と根拠

ORDレコード
ord-43d0344d68684cd3b55b16e4f49538b4
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187453B2

反応ノート

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