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Cyclohexylamine → 5-amino-2-cyclohexylamino-8-(3-hydroxy-propyl)-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 2386687
ノート
印刷プレビュー

反応式

HRID 2386687 の反応式
[NH2:1][C:2]1[C:11]2[CH:10]=[N:9][C:8](SC)=[N:7][C:6]=2[N:5]([CH2:14][CH2:15][CH2:16][O:17][Si](C(C)(C)C)(C)C)[C:4](=[O:25])[CH:3]=1.ClC1C=C(C=CC=1)C(OO)=O.[CH:37]1([NH2:43])[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]1>C(Cl)Cl>[NH2:1][C:2]1[C:11]2[CH:10]=[N:9][C:8]([NH:43][CH:37]3[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]3)=[N:7][C:6]=2[N:5]([CH2:14][CH2:15][CH2:16][OH:17])[C:4](=[O:25])[CH:3]=1
参加物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 7965CyclohexylamineHCID 70297m-Chloroperbenzoic acidHCID 579294635-amino-8-[3-(tert-butyl-dimethyl-silanyloxy)-propyl]-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 444643895-amino-2-cyclohexylamino-8-(3-hydroxy-propyl)-8H-pyrido[2,3-d]pyrimidin-7-one収率 23.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

To a solution of 5-amino-8-[3-(tert-butyl-dimethyl-silanyloxy)-propyl]-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one (150 mg, 0.395 mmol) in DCM (9 mL) was added 3-chloroperoxybenzoic acid (77% max., 106 mg, 0.474 mmol) at RT under argon atmosphere and the resulting mixture was stirred for 40 min. The reaction mixture was then evaporated under reduced pressure and the residue was dissolved in anhydrous dimethyl sulfoxide (ca. 9 mL). Cyclohexylamine (0.226 mL, 1.975 mmol) was then added at RT and the resulting mixture was stirred at 80° C. for 1.5 h. The reaction mixture was then quenched with water (70 mL) and an aqueous saturated solution of ammonium chloride (30 mL). The resulting mixture was extracted with EtOAc; the organic extracts were washed twice with water (50 mL), dried over MgSO4, filtered and evaporated under reduced pressure. To the residue, dissolved in THF, was added a solution of tetrabutylammonium fluoride (1 M in THF, 0.59 mL) at RT and the resulting mixture was stirred overnight. The solid formed was collected by filtration, washed with hexane and purified by preparative TLC (DCM/MeOH, 90/10) to give 30 mg of 5-amino-2-cyclohexylamino-8-(3-hydroxy-propyl)-8H-pyrido[2,3-d]pyrimidin-7-one as a yellow powder. MS=318 [M+H]+; MP=131.0-132.5° C.

後処理

  1. customThe reaction mixture was then evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in anhydrous dimethyl sulfoxide (ca. 9 mL)
  3. stirringthe resulting mixture was stirred at 80° C. for 1.5 h
  4. customThe reaction mixture was then quenched with water (70 mL)
  5. extractionThe resulting mixture was extracted with EtOAc
  6. washthe organic extracts were washed twice with water (50 mL)
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customevaporated under reduced pressure
  10. dissolutionTo the residue, dissolved in THF
  11. additionwas added a solution of tetrabutylammonium fluoride (1 M in THF, 0.59 mL) at RT
  12. stirringthe resulting mixture was stirred overnight
  13. customThe solid formed
  14. filtrationwas collected by filtration
  15. washwashed with hexane
  16. custompurified by preparative TLC (DCM/MeOH, 90/10)

出典と根拠

ORDレコード
ord-d1955aa888a442d39d399c6e0311a800
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268840B2

反応ノート

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