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Phosphorus oxychloride → 5,6-Dimethyl-2-(4-methylthiazol-2-yl)amino-4-chloropyrimidine

HRID 275926
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HRID 275926 반응식
[CH3:1][C:2]1[C:3](O)=[N:4][C:5]([NH:9][C:10]2[S:11][CH:12]=[C:13]([CH3:15])[N:14]=2)=[N:6][C:7]=1[CH3:8].P(Cl)(Cl)([Cl:19])=O>CN(C)C=O>[CH3:1][C:2]1[C:3]([Cl:19])=[N:4][C:5]([NH:9][C:10]2[S:11][CH:12]=[C:13]([CH3:15])[N:14]=2)=[N:6][C:7]=1[CH3:8]
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참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178431960HCID 178431960, 화합물

생성물 1

HCID 183156855,6-Dimethyl-2-(4-methylthiazol-2-yl)amino-4-chloropyrimidine수율 33.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The mixture solution of 5,6-dimethyl-2-(4-methylthiazol-2-yl)amino-4-hydroxypyrimidine (1.15 g, 4-78 mmol), phosphorus oxychioride(7 ml), and dimethylformamide(5 ml) was heated to 70° C. for 30 minutes, cooled to a room temperature and then poured into ice water. The aqueous layer was extracted with dichloromethane, washed with 1N sodium hydroxide solution, and then washed with water. The separated organic layer was concentrated and the residual oil was suspended in a mixture solution of ethyl ether and hexane. The resulting solid was filtered and dried to give 0.42 g of the titled compound. (Yield: 33.9%)

후처리

  1. extractionThe aqueous layer was extracted with dichloromethane
  2. washwashed with 1N sodium hydroxide solution
  3. washwashed with water
  4. concentrationThe separated organic layer was concentrated
  5. filtrationThe resulting solid was filtered
  6. customdried

출처 및 근거

ORD 기록
ord-8d5b275a824a498cbd117255cac1bb98
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06352993B1

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