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Acetone → 2-(2-chloro-9-methyl-6-morpholino-9H-purin-8-yl)propan-2-ol

HRID 1692681
ノート
印刷プレビュー

反応式

HRID 1692681 の反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH3:11])=[C:4]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[N:3]=1.C([Li])CCC.[CH3:23][C:24]([CH3:26])=[O:25]>C1COCC1>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[C:7]([C:24]([OH:25])([CH3:26])[CH3:23])[N:8]2[CH3:11])=[C:4]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[N:3]=1
参加物反応条件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 180AcetoneHCID 715006872-Chloro-9-methyl-6-(4-morpholinyl)-9H-purineHCID 178418339Butyllithium

生成物 1

HCID 580152132-(2-chloro-9-methyl-6-morpholino-9H-purin-8-yl)propan-2-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

4-(2-Chloro-9-methyl-9H-purin-6-yl)morpholine (233 mg) was cooled in 5 mL of anhydrous THF to −78° C. before adding 2 eq of a 2.5 M solution of n-butyl lithium. The reaction was stirred for 1 hour at −78° C. upon which 3 eq of acetone were added. The reaction was subsequently warmed to 0° C. after 30 minutes. The reaction was quenched with water and extracted with ethyl acetate. The organic layer was concentrated to give crude 2-(2-chloro-9-methyl-6-morpholino-9H-purin-8-yl)propan-2-ol (95 mg).

後処理

  1. additionwere added
  2. customThe reaction was quenched with water
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic layer was concentrated

出典と根拠

ORDレコード
ord-d720f5a3066a4322887747f4e4afccb8
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158624B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート