2-Chloroethyl isocyanate → 1-(2-Chloroethyl)-3-(3-methyl-4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)urea

HRID 1361698노트

반응식

HRID 1361698 반응식
[NH2:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][C:7]2[C:12]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([NH:19][CH3:20])[N:14]=3)=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:4]([CH3:23])[CH:3]=1.[Cl:24][CH2:25][CH2:26][N:27]=[C:28]=[O:29]>C1COCC1>[Cl:24][CH2:25][CH2:26][NH:27][C:28]([NH:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][C:7]2[C:12]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([NH:19][CH3:20])[N:14]=3)=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:4]([CH3:23])[CH:3]=1)=[O:29]

참가 물질

4

반응물 2

HCID 160352-Chloroethyl isocyanateHCID 469295424-(2-(4-amino-2-methylphenoxy)pyridin-3-yl)-N-methylpyrimidin-2-amine

생성물 1

HCID 669705851-(2-Chloroethyl)-3-(3-methyl-4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)urea

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a slurry of 4-(2-(4-amino-2-methylphenoxy)pyridin-3-yl)-N-methylpyrimidin-2-amine (0.500 g, 1.63 mmol) in THF (3.3 mL) under nitrogen was added 1-chloro-2-isocyanatoethane (0.157 mL, 1.79 mmol). The reaction became clear and brown, and then a precipitate formed. Additional THF (4 mL) was added to promote stirring, and the reaction was allowed to stir for 16 h. The mixture was filtered, the solid was rinsed with diethyl ether, and dried in vacuo to give 1-(2-chloroethyl)-3-(3-methyl-4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)urea as a tan solid. MS m/z=413 [M+1]+. Calc'd for C20H21ClN6O2: 412.14.

후처리

  1. custombrown, and then a precipitate formed
  2. stirringto stir for 16 h
  3. filtrationThe mixture was filtered
  4. washthe solid was rinsed with diethyl ether
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-f935e411e08e4e89a15337b9c905bc37
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07880000B2

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