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Diisopropylamine → N-cyclopentyl-4-[2-isobutyl-7-(methylthio)pyrazolo[1,5-a]pyridin-3-yl]pyrimidin-2-amine

HRID 859972
ノート
印刷プレビュー

反応式

HRID 859972 の反応式
[CH:1]1([NH:6][C:7]2[N:12]=[C:11]([C:13]3[C:14]([CH2:22][CH:23]([CH3:25])[CH3:24])=[N:15][N:16]4[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=34)[CH:10]=[CH:9][N:8]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.C([N-]C(C)C)(C)C.[Li+].C([Li])CCC.C(NC(C)C)(C)C.[CH3:46][S:47]SC>O1CCCC1.CCOCC.O>[CH:1]1([NH:6][C:7]2[N:12]=[C:11]([C:13]3[C:14]([CH2:22][CH:23]([CH3:25])[CH3:24])=[N:15][N:16]4[C:21]([S:47][CH3:46])=[CH:20][CH:19]=[CH:18][C:17]=34)[CH:10]=[CH:9][N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5]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

9

反応物 5

HCID 7912DiisopropylamineHCID 12232Dimethyl DisulfideHCID 2724682Lithium diisopropylamideHCID 10042600HCID 10042600、化合物HCID 178418339Butyllithium

生成物 1

HCID 10339828N-cyclopentyl-4-[2-isobutyl-7-(methylthio)pyrazolo[1,5-a]pyridin-3-yl]pyrimidin-2-amine

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a cold (−78° C.) solution of N-cyclopentyl-4(2-isobutylpyrazolo[1,5-a]pyridin-3-yl)pyrimidin-2-amine (750 mg, 2.23 mmol) in tetrahydrofuran (25 mL) was added lithium diisopropylamide (LDA) (11.18 mL of a 0.6 M stock solution was prepared from 18.75 mL of 1.6 M butyllithium and 4.20 mL of diisopropylamine in 27 mL of tetrahydrofuran, 6.71 mmol) dropwise. The reusitant solution was stirred at −78° C. for 15 minutes. Dimethyldisulfide (1.0 mL, 11.15 mmol) was added rapidly and the mixture was stirred for 1 hour. Water and ether were added and the layers separated. The organic layer was washed with brine. The aqueous layer was extracted with ether and the combined organics were dried over magnesium sulfate. Filtration and concentration followed flash chromatography on silica gel (2:1 hexane-ether) provided N-cyclopentyl-4-[2-isobutyl-7-(methylthio)pyrazolo[1,5-a]pyridin-3-yl]pyrimidin-2-amine. (712 mg, 84%) as a yellow solid. 1H NMR (CDCl3) δ 8.25 (d, 1H), 8.07 (d, 1H), 7.25 (t, 1H), 6.75 (d, 1H), 6.61 (d, 1H), 5.04 (d, 1H), 4.37 (m, 1H), 3.05 (d, 2H), 2.61 (s, 3H), 2.26–2.05 (m, 3H), 1.79–1.50 (m, 6H), 0.97 (d, 6H); MS m/z 382 (M+1).

後処理

  1. stirringthe mixture was stirred for 1 hour
  2. customthe layers separated
  3. washThe organic layer was washed with brine
  4. extractionThe aqueous layer was extracted with ether
  5. dry with materialthe combined organics were dried over magnesium sulfate
  6. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-bc2876a2aeea44738b7a6e096463c11e
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07153863B2

反応ノート

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