Hydrochloric Acid → Methyl 2-(1-(3,4-dichlorophenylsulfonyl)pyrrolidin-2-yl)acetate

HRID 1642143ノート

反応式

HRID 1642143 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].[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH:17]1[CH2:21][CH2:20][CH2:19][NH:18]1.Cl>C(Cl)Cl.C(N(CC)CC)C>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:18]2[CH2:19][CH2:20][CH2:21][CH:17]2[CH2:16][C:15]([O:14][CH3:13])=[O:22])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 5323862Methyl 2-(pyrrolidin-2-yl)acetate

生成物 1

HCID 66756029Methyl 2-(1-(3,4-dichlorophenylsulfonyl)pyrrolidin-2-yl)acetate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

実験手順

A solution of 3,4-dichlorobenzenesulfonyl chloride (1.88 g, 7.65 mmol) in DCM (15 ml) was added dropwise at 0° C. to a solution, cooled to 0° C., of pyrrolidin-2-ylacetic acid methyl ester (1.5 g, 8.4 mmol) in DCM (33 ml) and triethylamine was (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, 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: 2.1 g (77%)

後処理

  1. stirringstirring
  2. waitwas carried out for a further 15 minutes
  3. customThe organic phase was separated
  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-afc8ef7011c644f5a030ab3b2fe811ff
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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