2-Chloro-4-(trifluoromethyl)pyrimidine → HCID 67432560、化合物

HRID 1887090ノート

反応式

HRID 1887090 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH:5]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[CH:15]=[N:14][CH:13]=[CH:12]3)[CH2:4][CH2:3]1.[Cl:19][C:20]1[N:25]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:23]=[CH:22][N:21]=1>N1C=CC=CC=1.CN(C=O)C>[ClH:19].[F:27][C:26]([F:29])([F:28])[C:24]1[CH:23]=[CH:22][N:21]=[C:20]([N:2]2[CH2:7][CH2:6][CH:5]([O:8][C:9]3[CH:10]=[C:11]4[C:16](=[CH:17][CH:18]=3)[CH:15]=[N:14][CH:13]=[CH:12]4)[CH2:4][CH2:3]2)[N:25]=1

参加物

5

反応物 2

HCID 27739122-Chloro-4-(trifluoromethyl)pyrimidineHCID 674289666-(Piperidin-4-yloxy)-isoquinoline hydrochloride

生成物 1

HCID 67432560HCID 67432560、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

75 mg of 6-(Piperidine-4-yloxy)-isoquinoline-Hydrochloride (124) are dissolved in 5 mL of dry pyridine and 5 mL of DMF. 55 mg 2-Chlor-4-trifluoromethyl-pyrimidine are added and the solution is stirred at 60° C. for 3 hours. The solvents are removed in vacuo and the residue is taken up in brine and extracted three times with ethyl acetate. The combined organic layers are dried over magnesium sulfate, evaporated to dryness and the crude product is purified by preparative HPLC. The product is converted into the corresponding HCl salt by taking up the product in 20 mL of 1 N hydrochloric acid followed by lyophilization. Yield: 29 mg. Rt=1.69 min (Method #2). Detected mass: 375.1 (M+H+).

後処理

  1. customThe solvents are removed in vacuo
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic layers are dried over magnesium sulfate
  4. customevaporated to dryness
  5. customthe crude product is purified by preparative HPLC

出典と根拠

ORDレコード
ord-57a249dbc8784933a0d327387aed7f08
出典データセット
uspto-grants-2013_08
特許番号
US08501736B2

反応ノート

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