2-Chloro-4-(trifluoromethyl)pyrimidine → HCID 67432560, 화합물

HRID 1022880노트

반응식

HRID 1022880 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 67432560HCID 67432560, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-43d4cea4084d41378e74a735d4b02a4e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722671B2

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