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Hydrochloric Acid → HCID 67408461、化合物

HRID 1622189
ノート
印刷プレビュー

反応式

HRID 1622189 の反応式
[CH3:1][N:2]([CH3:25])[S:3]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:16][CH2:15][C@H:14]([NH:17]C(=O)OC(C)(C)C)[CH2:13]2)=[CH:8][CH:7]=1)(=[O:5])=[O:4].[ClH:26]>C(OCC)(=O)C>[ClH:26].[ClH:26].[NH2:17][C@H:14]1[CH2:15][CH2:16][N:12]([C:9]2[CH:8]=[CH:7][C:6]([S:3]([N:2]([CH3:25])[CH3:1])(=[O:4])=[O:5])=[CH:11][CH:10]=2)[CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 68236280HCID 68236280、化合物

生成物 1

HCID 67408461HCID 67408461、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

In ethyl acetate was dissolved 8.39 g of tert-butyl [(S)-1-(4-dimethylsulfamoylphenyl)-pyrrolidin-3-yl]carbamate, 200 ml of a solution of 4M hydrochloric acid in ethyl acetate was added thereto, and the mixture was stirred at room temperature for 3 days. The solvent was evaporated, and then, diethyl ether was added to the residue, and the precipitates were collected by filtration to obtain 4-[(S)-3-aminopyrrolidin-1-yl]-N,N-dimethyl-benzenesulfonamide dihydrochloride. To the 4-[(S)-3-aminopyrrolidin-1-yl]-N,N-dimethyl-benzenesulfonamide dihydrochloride were added a saturated aqueous sodium bicarbonate solution and chloroform, the mixture was stirred and the liquids were separated. The organic layer was dried and concentrated under reduced pressure to obtain 5.85 g of 4-[(S)-3-aminopyrrolidin-1-yl]-N,N-dimethyl-benzenesulfonamide.

後処理

  1. additionwas added
  2. customThe solvent was evaporated
  3. additiondiethyl ether was added to the residue
  4. filtrationthe precipitates were collected by filtration

出典と根拠

ORDレコード
ord-96b7648fe5ef46959102ebb2d7300a2c
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08778628B2

反応ノート

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