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Hydrochloric Acid → 5-Chloro-6-(2-chloro-4-fluorophenyl)-7-(4-methylpiperidin-1-yl)-3-methylmercapto-pyrazolo [2,3-a]pyrimidine

HRID 1866085
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HRID 1866085 반응식
[Cl-].[Cl-].[Cl-].[Al+3].[Cl:5][C:6]1[C:11]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=2[Cl:19])=[C:10]([N:20]2[CH2:25][CH2:24][CH:23]([CH3:26])[CH2:22][CH2:21]2)[N:9]2[N:27]=[CH:28][CH:29]=[C:8]2[N:7]=1.[CH3:30][S:31](OC)(=O)=S.Cl>ClCCl>[Cl:5][C:6]1[C:11]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=2[Cl:19])=[C:10]([N:20]2[CH2:25][CH2:24][CH:23]([CH3:26])[CH2:22][CH2:21]2)[N:9]2[N:27]=[CH:28][C:29]([S:31][CH3:30])=[C:8]2[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6451240Aluminum(III) ChlorideHCID 14573333Methyl methylthiosulphonateHCID 866003145-Chloro-6-(2-chloro-4-fluorophenyl)-7-(4-methylpiperidin-1-yl)pyrazolo[2,3-a]pyrimidine

생성물 1

HCID 579774485-Chloro-6-(2-chloro-4-fluorophenyl)-7-(4-methylpiperidin-1-yl)-3-methylmercapto-pyrazolo [2,3-a]pyrimidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

With stirring, 1.06 g of aluminium trichloride were initially added to 1 g of 5-chloro-6-(2-chloro-4-fluorophenyl)-7-(4-methylpiperidin-1-yl)pyrazolo[2,3-a]pyrimidine, the preparation of which is described, for example, in WO 02/048151, in 50 ml of dichloromethane, and 0.99 g of methyl methylthiosulphonate was then added dropwise. After 15 h of stirring at room temperature, the mixture was poured into ice-water and hydrochloric acid was added. The organic phase was separated off, and the aqueous phase was extracted two more times with in each case 15 ml of ethyl acetate. The combined organic phases were dried with sodium sulphate, and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel using cyclohexane/ethyl acetate 4:1. This gave 0.65 g of an orange oil, logPs=5.73.

후처리

  1. customthe preparation of which
  2. stirringAfter 15 h of stirring at room temperature
  3. additionwas added
  4. customThe organic phase was separated off
  5. extractionthe aqueous phase was extracted two more times with in each case 15 ml of ethyl acetate
  6. dry with materialThe combined organic phases were dried with sodium sulphate
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-9999fd6842d74a18972790ed93266ef8
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07629294B2

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