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Ammonia → 2-{4-[3-(N,N-Dimethyl)amino-2-hydroxypropoxy]anilino}-4-(2,4-difluoroanilino)pyrimidine

HRID 347736
ノート
印刷プレビュー

反応式

HRID 347736 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[F:16])[CH:5]=[CH:4][N:3]=1.Cl.[CH3:18][N:19]([CH2:21][CH:22]([OH:32])[CH2:23][O:24][C:25]1[CH:31]=[CH:30][C:28]([NH2:29])=[CH:27][CH:26]=1)[CH3:20].CO.N>C(O)CCC>[CH3:20][N:19]([CH2:21][CH:22]([OH:32])[CH2:23][O:24][C:25]1[CH:26]=[CH:27][C:28]([NH:29][C:2]2[N:7]=[C:6]([NH:8][C:9]3[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=3[F:16])[CH:5]=[CH:4][N:3]=2)=[CH:30][CH:31]=1)[CH3:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 887MethanolHCID 179811362-Chloro-4-(2,4-difluoroanilino)pyrimidineHCID 227319204-[2-hydroxy-3-(N,N-dimethylamino)propoxy]aniline hydrochloride

生成物 1

HCID 210837252-{4-[3-(N,N-Dimethyl)amino-2-hydroxypropoxy]anilino}-4-(2,4-difluoroanilino)pyrimidine収率 41.5%

試薬・触媒・溶媒 1

HCID 263
1-Butanol
溶媒

反応条件

温度
100 °C

実験手順

2-Chloro-4-(2,4-difluoroanilino)pyrimidine (Reference Example A-2; 174 mg, 0.72 mmol) was dissolved in n-butanol (2 ml) and 4-[3-(N,N-dimethyl)amino-2-hydroxypropoxy]aniline hydrochloride (Reference Example D-1; 198 mg, 0.72 mmol) was added. The resulting suspension was treated with methanol until all the solid dissolved. The reaction mixture was heated at 100° C. for 12 hours and allowed to cool to ambient temperature. The reaction mixture was then basified to pH 9–10 using methanolic ammonia and evaporated onto silica (5 ml). The residue was purified by column chromatography eluting with methanol (15%): DCM:aqueous ammonia(1%). The resulting gum was recrystallized from acetonitrile to give the title product as a solid (124 mg, 41%). NMR (300 MHz): 2.18 (s, 6H), 2.34 (m, 2H), 3.78 (m, 1H), 3.88 (m, 2H), 4.75 (brd, 1H), 6.18 (d, 1H), 6.75 (d, 2H), 7.03 (t, 1H), 7.32 (t, 1H), 7.48 (d, 2H), 7.88 (dd, 1H), 7.95 (d, 1H), 8.88 (s, 1H), 8.95(s, 1H); m/z: (ES+) 416.4 (MH+).

後処理

  1. dissolutiondissolved
  2. temperatureto cool to ambient temperature
  3. customevaporated onto silica (5 ml)
  4. customThe residue was purified by column chromatography
  5. washeluting with methanol (15%)
  6. customThe resulting gum was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-b755efa91aaf4546addb480a8da43398
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176212B2

反応ノート

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