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Tert-Butylamine → HCID 10127447、化合物

HRID 1296728
ノート
印刷プレビュー

反応式

HRID 1296728 の反応式
[CH:1]1([NH:6][C:7]2[N:12]=[C:11]([C:13]3[C:14]([C:24]4[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=4)=[N:15][N:16]4[C:21]=3[CH:20]=[CH:19][N:18]=[C:17]4SC)[CH:10]=[CH:9][N:8]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.ClC1C=C(C=CC=1)C(OO)=O.[C:42]([NH2:46])([CH3:45])([CH3:44])[CH3:43]>ClCCl.O>[C:42]([NH:46][C:17]1[N:16]2[N:15]=[C:14]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[C:13]([C:11]3[CH:10]=[CH:9][N:8]=[C:7]([NH:6][CH:1]4[CH2:2][CH2:3][CH2:4][CH2:5]4)[N:12]=3)=[C:21]2[CH:20]=[CH:19][N:18]=1)([CH3:45])([CH3:44])[CH3:43]
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 3

HCID 6385Tert-Butylamine2 回HCID 70297m-Chloroperbenzoic acid2 回HCID 10173307HCID 10173307、化合物

生成物 1

HCID 10127447HCID 10127447、化合物収率 14%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6344
Dichloromethane
溶媒
2 回

実験手順

To a solution of N-cyclopentyl-4-[2-(4-fluorophenyl)-7-(methylsulfanyl)pyrazolo[1,5-c]pyrimidin-3-yl]pyrimidin-2-amine (40 mg, 0.095 mmol) in dichloromethane (2 mL) was added 3-chloroperoxybenzoic acid (12 mg, 0.14 mmol) and the reaction mixture stirred at room temperature for 1 hour. t-Butylamine (3 mL) was added and heated to reflux for 3 hours. The reaction was allowed to cool and diluted with water. The mixture was extracted with ethyl acetate and the organic phase washed with brine before being concentrated under vacuum. The residue was purified by silica gel chromatography eluting with SO/5 acetone in dichloromethane to yield a 1:1 mixture of starting material and product. The residue was dissolved in dichloromethane (2 mL) and 3-chloroperoxybenzoic acid (18 mg, 0.21 mmol) was added. The mixture was stirred for 2 hours and then t-butylamine (3 mL) was added. The reaction mixture was stirred for 3 hours, diluted with water, extracted with ethyl acetate, washed with brine, concentrated, and the residue purified by silica gel chromatography eluting with 5% acetone in dichloromethane to yield N-(tert-butyl)-3-[2-(cyclopentylamino)pyrimidin-4-yl]-2-(4-fluorophenyl)pyrazolo[1,5-c]pyrimidin-7-amine (6 mg, 14%), 1H NMR (CDCl3): δ 8.02 (d, 1H), 7.72 (d, 1H), 7.60 (dd, 2H), 7.47 (d, 1H), 7.13 (t, 2H), 6.42 (s, 1H), 6.25 (d, 1H), 5.14 (bs, 1H), 4.28 (m, 1H), 2.04 (m, 2H), 1.45–1.78 (m, 15H). MS m/z 446 (M+1).

後処理

  1. temperatureheated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe organic phase washed with brine
  6. concentrationbefore being concentrated under vacuum
  7. customThe residue was purified by silica gel chromatography
  8. washeluting with SO/5 acetone in dichloromethane
  9. customto yield
  10. additiona 1:1 mixture of starting material and product
  11. stirringThe mixture was stirred for 2 hours
  12. stirringThe reaction mixture was stirred for 3 hours
  13. extractionextracted with ethyl acetate
  14. washwashed with brine
  15. concentrationconcentrated
  16. customthe residue purified by silica gel chromatography
  17. washeluting with 5% acetone in dichloromethane

出典と根拠

ORDレコード
ord-7ad20545356c41f8babf54f49094a4ff
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07247626B2

反応ノート

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