Isopropenyl chloroformate → Prop-1-en-2-yl (2-fluoro-4-methyl-5-(7-methyl-2-(methylamino)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate

HRID 522728노트

반응식

HRID 522728 반응식
[NH2:1][C:2]1[C:3]([F:22])=[CH:4][C:5]([CH3:21])=[C:6]([C:8]2[C:19]([CH3:20])=[N:18][C:11]3[N:12]=[C:13]([NH:16][CH3:17])[N:14]=[CH:15][C:10]=3[CH:9]=2)[CH:7]=1.Cl[C:24]([O:26][C:27]([CH3:29])=[CH2:28])=[O:25]>N1C=CC=CC=1>[F:22][C:3]1[CH:4]=[C:5]([CH3:21])[C:6]([C:8]2[C:19]([CH3:20])=[N:18][C:11]3[N:12]=[C:13]([NH:16][CH3:17])[N:14]=[CH:15][C:10]=3[CH:9]=2)=[CH:7][C:2]=1[NH:1][C:24](=[O:25])[O:26][C:27]([CH3:29])=[CH2:28]

참가 물질

4

반응물 2

HCID 93846Isopropenyl chloroformateHCID 898135606-(5-Amino-4-fluoro-2-methylphenyl)-N,7-dimethylpyrido[2,3-d]pyrimidin-2-amine

생성물 1

HCID 118048014Prop-1-en-2-yl (2-fluoro-4-methyl-5-(7-methyl-2-(methylamino)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate수율 100%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
0 °C

실험 절차

Treat a cooled solution (0° C.) of 6-(5-amino-4-fluoro-2-methylphenyl)-N,7-dimethylpyrido[2,3-d]pyrimidin-2-amine (0.85 g, 2.86 mmol) in pyridine (10 mL) dropwise with isopropenyl chloroformate (0.281 ml, 2.57 mmol) and stir the mixture for 20 min. at 0° C. Concentrate the mixture to dryness, dissolve the residue in DCM, wash with brine, dry over Na2SO4 and concentrate to dryness to afford the title compound. Use it without purification (assuming 100% yield). MS (m/z): 382.1 (M+1).

후처리

  1. concentrationConcentrate the mixture to dryness
  2. dissolutiondissolve the residue in DCM
  3. washwash with brine
  4. dry with materialdry over Na2SO4
  5. concentrationconcentrate to dryness

출처 및 근거

ORD 기록
ord-38ce905859d74b3baf6a9dc752227a7a
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334267B2

반응 노트

불러오는 중…