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Chlorosuccinimide → 4-(4-Chloro-5-(2,5-dimethyl-7-(pentan-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)thiazol-2-yl)morpholine

HRID 1660747
ノート
印刷プレビュー

反応式

HRID 1660747 の反応式
Br[C:2]1[N:3]=[C:4]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[S:5][C:6]=1[C:7]1[C:8]([CH3:22])=[N:9][N:10]2[C:15]([CH:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][C:13]([CH3:21])=[N:12][C:11]=12.C([Li])CCC.[Cl:34]N1C(=O)CCC1=O.[Cl-].N>C1COCC1>[Cl:34][C:2]1[N:3]=[C:4]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[S:5][C:6]=1[C:7]1[C:8]([CH3:22])=[N:9][N:10]2[C:15]([CH:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][C:13]([CH3:21])=[N:12][C:11]=12
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

6

反応物 4

HCID 31398ChlorosuccinimideHCID 20976574Ammonia chlorideHCID 67428983HCID 67428983、化合物HCID 178418339Butyllithium

生成物 1

HCID 248989774-(4-Chloro-5-(2,5-dimethyl-7-(pentan-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)thiazol-2-yl)morpholine収率 51.4%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
-78 °C

実験手順

Under a nitrogen atmosphere dissolve 3-(4-bromo-2-morpholin-4-yl-thiazol-5-yl)-7-(1-ethyl-propyl)-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (116 mg, 0.25 mmol) in THF (1.5 mL) and chill to −78° C. Add n-butyl lithium (0.1 mL. 2.5 M in hexane, 0.25 mmol) and stir at −78° C. for 30 min. Add N-chlorosuccinimide (33.4 mg, 0.25 mmol) and stir for another 30 min, slowly warming to room temperature. After stirring overnight, quench the reaction by adding a solution of saturated ammonia chloride and extract with ethyl acetate. Wash the organic layer with brine, dry over sodium sulfate, filter, and concentrate to a residue. Purify the crude material by flash chromatography, eluting with hexanes:dichloromethane:ethyl acetate (5:5:2) to provide the title compound (54 mg). MS (APCI) m/z (35Cl) 420.6 (M+1)+; 1H NMR (400 MHz, CDCl3): 6.44 (s, 1H), 3.79 (t, 4H, J=4.8 Hz), 3.63-3.56 (m, 1H), 3.47 (t, 4H, J=4.8 Hz), 2.55 (s, 3H), 2.45 (s, 3H), 1.88-1.75 (m, 4H), 0.87 (t, 6H, J=7.5 Hz).

後処理

  1. temperatureslowly warming to room temperature
  2. customquench
  3. customthe reaction
  4. extractionextract with ethyl acetate
  5. washWash the organic layer with brine
  6. dry with materialdry over sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate to a residue
  9. customPurify the crude material by flash chromatography
  10. washeluting with hexanes:dichloromethane:ethyl acetate (5:5:2)

出典と根拠

ORDレコード
ord-e6c51a9b595947268f6845f46b1dc5dd
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030304B2

反応ノート

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