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N,N-Diethylaniline → 4-Chloro-6-methoxy-2-(4-trifluoromethyl-thiazol-2-yl)-pyrimidine

HRID 530743
ノート
印刷プレビュー

反応式

HRID 530743 の反応式
O[C:2]1[N:7]=[C:6]([C:8]2[S:9][CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[N:12]=2)[NH:5][C:4]([O:18][CH3:19])(O)[CH:3]=1.C(N(CC)C1C=CC=CC=1)C.O=P(Cl)(Cl)[Cl:33]>>[Cl:33][C:2]1[CH:3]=[C:4]([O:18][CH3:19])[N:5]=[C:6]([C:8]2[S:9][CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[N:12]=2)[N:7]=1
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

4

反応物 3

HCID 7061N,N-DiethylanilineHCID 24813Phosphorus oxychlorideHCID 178494417HCID 178494417、化合物

生成物 1

HCID 582826704-Chloro-6-methoxy-2-(4-trifluoromethyl-thiazol-2-yl)-pyrimidine収率 45%

反応条件

温度
110 °C

実験手順

To a stirred solution of compound 289 (2.38 g, 1 eq.) in POCl3 (7.2 mL) was added N,N-diethylaniline (2.17 g, 1.7 eq.). The mixture was stirred at 110° C. for 16 hrs. The reaction was cooled down to room temperature and poured dropwise into an ice/water mixture. The aqueous solution was extracted with DCM. Organics were dried over Na2SO4, filtered, concentrated under reduced pressure, and purified by silica gel chromatography to yield compound 290 as an orange solid in 45% yield. MS (ESI, EI+): m/z=296 (MH+).

後処理

  1. temperatureThe reaction was cooled down to room temperature
  2. extractionThe aqueous solution was extracted with DCM
  3. dry with materialOrganics were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-2d3e4a54199d46eb9477ddc36e14d72d
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353100B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート