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

HRID 1418003
ノート
印刷プレビュー

反応式

HRID 1418003 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

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.;

後処理

  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

出典と根拠

ORDレコード
ord-ec0594f0a7b744acba96a7c5119e8fe2
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05880130

反応ノート

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