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Dimethylamine → 4-[3'-(3-Dimethylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino)pyrimidine

HRID 1418003
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HRID 1418003 반응식
[O:1]1[CH2:26][CH:2]1[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:23]=[CH:24][CH:25]=1)[NH:8][C:9]1[CH:14]=[C:13]([NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[N:12]=[CH:11][N:10]=1.[CH3:27][NH:28][CH3:29]>C(O)C.CN(C=O)C.O>[CH3:27][N:28]([CH3:29])[CH2:26][CH:2]([OH:1])[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:23]=[CH:24][CH:25]=1)[NH:8][C:9]1[CH:14]=[C:13]([NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[N:12]=[CH:11][N:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 674DimethylamineHCID 867538554-[3'-(2,3-Epoxypropoxy)anilino]6-(3'-methylanilino) pyrimidine

생성물 1

HCID 701859524-[3'-(3-Dimethylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino)pyrimidine수율 55%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

Using an analogous reaction procedure to that described in Example 33, a mixture of 4-[3'-(2,3-epoxypropoxy)anilino]6-(3'-methylanilino) pyrimidine, 33% dimethylamine in ethanol and DMF was stirred overnight at ambient temperature. The reaction mixture was diluted with water and extracted with ethyl acetate. The product so obtained was washed with water and with brine, dried (MgSO4) and evaporated. The residue was recrystallised from a mixture of methylene chloride, methanol and hexane to give 4-[3'-(3-dimethylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino)pyrimidine in 55% yield, m.p. 120°-122° C.;

후처리

  1. customan analogous reaction procedure to
  2. extractionextracted with ethyl acetate
  3. customThe product so obtained
  4. washwas washed with water and with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe residue was recrystallised from a mixture of methylene chloride, methanol and hexane

출처 및 근거

ORD 기록
ord-ec0594f0a7b744acba96a7c5119e8fe2
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05880130

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