Ethyl Acetate → 5-chloro-N-(2-(isopropylthio)phenyl)-3-(4-methoxybenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-7-amine

HRID 2046996노트

반응식

HRID 2046996 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[N:10]=[N:9][N:8]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=3)[C:6]=2[N:7]=1.[CH:21]([S:24][C:25]1[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=1[NH2:27])([CH3:23])[CH3:22].C(OCC)(=O)C>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:27][C:26]2[CH:28]=[CH:29][CH:30]=[CH:31][C:25]=2[S:24][CH:21]([CH3:23])[CH3:22])[C:5]2[N:10]=[N:9][N:8]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=3)[C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 138527202-(Isopropylthio)anilineHCID 582908695,7-dichloro-3-(4-methoxybenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine

생성물 1

HCID 582908655-chloro-N-(2-(isopropylthio)phenyl)-3-(4-methoxybenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-7-amine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 5,7-dichloro-3-(4-methoxybenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine (0.03 g) and 2-(isopropylthio)aniline (0.1 g) in dioxane (10 mL) was heated at 100° C. for 10 h. It was then cooled down to room temperature and ethyl acetate (20 mL) was added. The mixture was washed with saturated sodium bicarbonate (10 mL), and dried over sodium sulfate. Solvent was removed under reduced pressure and the remaining residue was purified on a silica gel column (ethyl acetate:hexane=1:10) to give desired product. ESMS calculated for C21H21ClN6OS (m/z): 440.1; found (M+H+): 441.1.

후처리

  1. washThe mixture was washed with saturated sodium bicarbonate (10 mL)
  2. dry with materialdried over sodium sulfate
  3. customSolvent was removed under reduced pressure
  4. customthe remaining residue was purified on a silica gel column (ethyl acetate:hexane=1:10)

출처 및 근거

ORD 기록
ord-85a7ec4f5ee44b7eba47caf3c9346bb3
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592432B2

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