1-Butanol → HCID 11294944, 화합물

HRID 411290노트

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HRID 411290 반응식
Cl[C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][C:6](C)=[C:7](C)[CH:8]=2)[N:3]=1.[CH2:15]([N:22]1[CH2:27][CH2:26][C:25]([CH2:34][NH:35][CH3:36])([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[C:37](=[O:40])([O-])[O-].[K+].[K+].[CH2:43]([OH:47])CCC>>[CH2:15]([N:22]1[CH2:23][CH2:24][C:25]([CH2:34][N:35]([CH3:36])[C:2]2[N:11]=[C:10]([NH2:12])[C:9]3[C:4](=[CH:5][C:6]([O:40][CH3:37])=[C:7]([O:47][CH3:43])[CH:8]=3)[N:3]=2)([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:26][CH2:27]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

5

반응물 4

HCID 2631-ButanolHCID 11430Potassium CarbonateHCID 11426409HCID 11426409, 화합물HCID 185407744-Amino-2-chloro-6,7-dimethylquinazoline

생성물 1

HCID 11294944HCID 11294944, 화합물

실험 절차

A mixture of 2-chloro-6,7-dimethyl-quinazolin-4-ylamine 1 (X=Cl) (900 mg), (1-benzyl-4-phenyl-piperidin-4-ylmethyl)-methyl-amine 2a (R1=CH3 and R2=phenyl) (440 mg) and potassium carbonate (250 mg) in 1-butanol (20 ml) was refluxed for 18 hours. The cooled reaction mixture was filtered, the filtrate was evaporated, and the residue was distributed between water and dichloromethane. The organic phase was dried over potassium carbonate, filtered, and evaporated. The residue was purified by flash chromatography on silica gel to provide 1.3 g of N2-(1-Benzyl-4-phenyl-piperidin-4-ylmethyl)-6,7-dimethoxy-N2-methyl-quinazoline-2,4-diamine 10, as an oil, MS: 485 (M+).

후처리

  1. customThe cooled reaction mixture
  2. filtrationwas filtered
  3. customthe filtrate was evaporated
  4. dry with materialThe organic phase was dried over potassium carbonate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-bf6a08d9250a42e684b2ac02f805af77
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559153B2

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