Ammonia → (RS)-S-{4-[(5-bromo-4-chloropyrimidin-2-yl)amino]phenyl}-S-methyl sulfoximide

HRID 1391468노트

반응식

HRID 1391468 반응식
[Br:1][C:2]1[C:3](O)=[N:4][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[NH:17])=[O:16])=[CH:11][CH:10]=2)=[N:6][CH:7]=1.N.P(Cl)(Cl)([Cl:23])=O>>[Br:1][C:2]1[C:3]([Cl:23])=[N:4][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[NH:17])=[O:16])=[CH:11][CH:10]=2)=[N:6][CH:7]=1

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 178504584HCID 178504584, 화합물

생성물 1

HCID 59674032(RS)-S-{4-[(5-bromo-4-chloropyrimidin-2-yl)amino]phenyl}-S-methyl sulfoximide

반응 조건

온도
106 °C

실험 절차

255 mg of (RS)-S-{4-[(5-bromo-4-hydroxypyrimidin-2-yl)amino]phenyl}-S-methyl sulfoximide is suspended in 1.5 ml of phosphorus oxychloride and stirred for 3 hours at 106° C. and for 16 hours at room temperature. The mixture is poured into ice water, made alkaline with 25% ammonia solution while being cooled intensely (temperature <5° C.) and stirred for 1 hour in an ice bath. The precipitate is suctioned off, washed with water and dried at 60° C. 220 mg (81.8% of theory) of the product with a melting point of 170-173° C. is obtained.

후처리

  1. temperaturewhile being cooled intensely (temperature <5° C.)
  2. stirringstirred for 1 hour in an ice bath
  3. washwashed with water
  4. customdried at 60° C
  5. custom220 mg (81.8% of theory) of the product with a melting point of 170-173° C. is obtained

출처 및 근거

ORD 기록
ord-19500b27f02a4ffaa1d81119156d1c75
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07338958B2

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