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Hydrochloric Acid → N-{4-[2-(4-aminophenyl)-7-(butylamino)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-butylamine

HRID 861118
ノート
印刷プレビュー

反応式

HRID 861118 の反応式
[CH2:1]([NH:5][C:6]1[N:11]2[N:12]=[C:13]([C:26]3[CH:31]=[CH:30][C:29]([N:32]=C(C4C=CC=CC=4)C4C=CC=CC=4)=[CH:28][CH:27]=3)[C:14]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([NH:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:16]=3)=[C:10]2[CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].Cl.CCOCC.C(=O)(O)[O-].[Na+]>O1CCCC1>[NH2:32][C:29]1[CH:28]=[CH:27][C:26]([C:13]2[C:14]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([NH:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:16]=3)=[C:10]3[CH:9]=[CH:8][CH:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:11]3[N:12]=2)=[CH:31][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 516892Sodium BicarbonateHCID 57444722HCID 57444722、化合物

生成物 1

HCID 10113479N-{4-[2-(4-aminophenyl)-7-(butylamino)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-butylamine

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of N-butyl-3-[2-(butylamino)-4-pyrimidinyl]-2-{4-[(diphenylmethylene)-amino]phenyl}pyrazolo[1,5-a]pyridin-7-amine (1.0 g, 1.7 mmol) in tetrahydrofuran (50 mL) was added hydrochloric acid (10 mL, 4 N aqueous). The resultant solution was stirred at room temperature for 30 minutes. Ether was added and the solution was made basic by the slow addition of saturated aqueous sodium bicarbonate. The organic layer was washed with brine. The aqueous layer was extracted with ether and the combined organics dried over magnesium sulfate. Filtration and concentration followed by flash chromatography (1:1 hexanes:ethyl acetate) provided N-{4-[2-(4-aminophenyl)-7-(butylamino)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-butylamine as an orange oil. 1H NMR (CDCl3): δ 8.02 (d, 1 H), 7.81 (d, 1 H), 7.47 (d, 2 H), 7.31 (m, 1 H), 6.77 (d, 2 H), 6.42 (d, 1 H), 6.08 (m, 1 H), 6.00 (d, 1 H), 5.18 (broad, 1 H), 3.86 (broad, 2 H), 3.53 (m, 2 H), 3.39 (m, 2 H), 1.82–1.64 (m, 4 H), 1.58–1.46 (m, 4 H), 1.04–0.99 (m, 6 H); MS m/z430 (M+1). This material was treated with anhydrous hydrochloric acid in ether to provide the corresponding hydrochloride salt.

後処理

  1. washThe organic layer was washed with brine
  2. extractionThe aqueous layer was extracted with ether
  3. dry with materialthe combined organics dried over magnesium sulfate
  4. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-e63f88e91837491f958dd067bc6a3f23
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07153855B2

反応ノート

読み込み中…

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