Hydrochloric Acid → 5-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

HRID 548947

반응식

HRID 548947 반응식
CC1C=C[C:5]([S:8]([N-]Cl)(=O)=O)=CC=1.O.O.O.[Na+].Cl.[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29](C)=[CH:28][C:27]=2S)=[N:23][CH:24]=1>C(#N)C.C(OCC)(=O)C>[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29]([S:8][CH3:5])=[CH:28][CH:27]=2)=[N:23][CH:24]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 517414chloramine-T trihydrateHCID 1317288425-Bromo-n4-isopropyl-n2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine

생성물 1

HCID 596740705-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

1.36 g (4.8 mmol) of chloramine-T trihydrate (Aldrich) are added to a suspension of 1.56 g (4.0 mmol) of the hydrochloride of 5-bromo-N4-isopropyl-N2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine in 20 ml of acetonitrile at room temperature. The mixture is stirred at room temperature for 16 hours and then diluted with ethyl acetate. The mixture is filtered with suction and the filter cake is washed with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated. The resulting residue is purified by HPLC:

후처리

  1. filtrationThe mixture is filtered with suction
  2. washthe filter cake is washed with ethyl acetate
  3. dry with materialThe combined organic phases are dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is purified by HPLC

출처 및 근거

ORD 기록
ord-038419359e4a4eff90deb757ec39e87f
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943629B2

연결된 노트

불러오는 중…