p-Toluenesulfonic acid monohydrate → 4-Methoxycarbonyl-4-phenylpiperidine p-toluenesulfonate

HRID 355462

反応式

HRID 355462 の反応式
O.[C:2]1([CH3:12])[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[C:13]1(C)C=CC(S(O)(=O)=O)=CC=1.[C:24]([C:27]1([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)([OH:26])=[O:25]>CO>[C:2]1([CH3:12])[CH:3]=[CH:4][C:5]([S:8]([OH:11])(=[O:9])=[O:10])=[CH:6][CH:7]=1.[CH3:13][O:25][C:24]([C:27]1([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:28][CH2:29][NH:30][CH2:31][CH2:32]1)=[O:26]

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 27236574-Piperidinecarboxylic acid, 4-phenyl-, 4-methylbenzenesulfonate (1:1)

生成物 1

HCID 216995184-Methoxycarbonyl-4-phenylpiperidine p-toluenesulfonate収率 453.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1 g of p-toluenesulphonic acid monohydrate is added to a solution of 10 g of 4-carboxy-4-phenylpiperidine p-toluenesulphonate in 300 ml of MeOH, and the reaction mixture is heated to reflux for 3 days. It is concentrated under vacuum, the residue is taken up in acetone and ether is added until precipitation takes place. After draining of the precipitate formed, 9.34 g of the expected product are obtained.

後処理

  1. temperaturethe reaction mixture is heated
  2. temperatureto reflux for 3 days
  3. concentrationIt is concentrated under vacuum
  4. additionether is added until precipitation
  5. customformed

出典と根拠

ORDレコード
ord-1f039885973f400ab1f5df807ddab499
出典データセット
uspto-grants-1998_11
特許番号
US05830906

関連ノート

読み込み中…