p-Toluenesulfonic acid → p-Toluenesulfonic acid

HRID 1463034ノート

反応式

HRID 1463034 の反応式
[S:1]1[C:5]2([CH2:9][C@@H:8]([C:10]([OH:12])=[O:11])[NH:7][CH2:6]2)[S:4][CH2:3][CH2:2]1.[CH3:13][C:14]1[CH:15]=[CH:16][C:17]([S:20]([OH:23])(=[O:22])=[O:21])=[CH:18][CH:19]=1.[C:24]1([C:30]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[N+]=[N-])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CN(C)C=O>[S:1]1[C:5]2([CH2:9][C@@H:8]([C:10]([O:12][CH:30]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[O:11])[NH:7][CH2:6]2)[S:4][CH2:3][CH2:2]1.[CH3:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([OH:23])(=[O:22])=[O:21])=[CH:16][CH:15]=1

参加物

6

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 612301,1'-(Diazomethylene)bis(benzene)HCID 128113941,4-Dithia-7-azaspiro[4.4]nonane-8-carboxylic acid, (8S)-

生成物 2

HCID 6101p-Toluenesulfonic acidHCID 86739577(S)-1,4-dithia-7-azaspiro[4.4]nonane-8-carboxylic acid, diphenylmethyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of (S)-1,4-dithia-7-azaspiro[4.4]nonane-8-carboxylic acid, p-toluenesulfonate (6.0 g.) in 30 ml. of anhydrous dimethylformamide at 50 ° under argon is added a dimethylformamide solution of diphenyldiazomethane (3.6) portionwise. After 10 minutes at 50°, the solvent is removed under reduced pressure. The residue is dissolved in ethyl acetate and precipitated with ether. The solvent is then decanted and the residue triturated with ethyl acetate/ether to give (S)-1,4-dithia-7-azaspiro [4.4]nonane-8-carboxylic acid, diphenylmethyl ester, p-toluenesulfonate.

後処理

  1. customthe solvent is removed under reduced pressure
  2. dissolutionThe residue is dissolved in ethyl acetate
  3. customprecipitated with ether
  4. customThe solvent is then decanted
  5. customthe residue triturated with ethyl acetate/ether

出典と根拠

ORDレコード
ord-0b6fe97c5b3a4b8c9c85d8aa5b7da39f
出典データセット
uspto-grants-1984_07
特許番号
US04462943

反応ノート

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