Hydrochloric Acid → HCID 66755784、化合物

HRID 1642146ノート

反応式

HRID 1642146 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.[CH3:14][O:15][C:16](=[O:24])[CH2:17][CH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][NH:19]1.C(N(CC)CC)C.Cl>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:19]2[CH2:20][CH2:21][CH2:22][CH2:23][CH:18]2[CH2:17][C:16]([O:15][CH3:14])=[O:24])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 8471TriethylamineHCID 13778732Methyl 2-(piperidin-2-yl)acetate hydrochloride

生成物 1

HCID 66755784HCID 66755784、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 3,4-dichlorobenzenesulfonyl chloride (1.88 g, 7.65 mmol) in DCM (15 ml) was added at 0° C. to a solution, cooled to 0° C., of piperidin-2-ylacetic acid methyl ester hydrochloride (1.3 g, 8.4 mmol) in DCM (33 ml) and triethylamine (2.66 ml, 21 mmol), and stirring was then carried out for 90 minutes at room temperature. 0.5 M HCl (20 ml) was then added, and stirring was carried out for a further 15 minutes. The organic phase was separated off, washed with water and dried over sodium sulfate. The solvent was removed using a rotary evaporator and the product was used in the next stage without being purified further. Yield: 1.9 g (63%)

後処理

  1. stirringstirring
  2. waitwas carried out for a further 15 minutes
  3. customThe organic phase was separated off
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed
  7. customa rotary evaporator
  8. customwithout being purified further

出典と根拠

ORDレコード
ord-623a01e4931f4c1984e51264e9a356a6
出典データセット
uspto-grants-2012_02
特許番号
US08119633B2

反応ノート

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