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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
ノート
印刷プレビュー

反応式

HRID 1866085 の反応式
[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
参加物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 313Hydrochloric AcidHCID 6451240Aluminum(III) ChlorideHCID 14573333Methyl methylthiosulphonateHCID 866003145-Chloro-6-(2-chloro-4-fluorophenyl)-7-(4-methylpiperidin-1-yl)pyrazolo[2,3-a]pyrimidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9999fd6842d74a18972790ed93266ef8
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07629294B2

反応ノート

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