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Methylamine → 4-[3'-(3-Methylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino) pyrimidine

HRID 1418005
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HRID 1418005 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][NH2:28]>C(O)C.O>[CH3:27][NH:28][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

5

반응물 2

HCID 6329MethylamineHCID 867538554-[3'-(2,3-Epoxypropoxy)anilino]6-(3'-methylanilino) pyrimidine

생성물 1

HCID 701870144-[3'-(3-Methylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino) pyrimidine수율 46%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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 and 33% methylamine in ethanol and NHP was stirred over 2 days at room 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-methylamino-2-hydroxypropoxy)anilino]6-(3'-methylanilino) pyrimidine is 46% yield, m.p. 88°-90° 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-7907808590f3499f9926e9f19ec97b8c
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05880130

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