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p-Toluenesulfonic acid → Almokalant

HRID 974191
ノート
印刷プレビュー

反応式

HRID 974191 の反応式
[CH2:1]([N:3]([CH2:17][CH2:18][CH2:19][S:20][CH2:21][CH2:22][CH3:23])[CH2:4][CH:5]([OH:16])[CH2:6][O:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1)[CH3:2].C1(C)C=CC(S(O)(=O)=[O:31])=CC=1.ClC1C=CC=C(C(OO)=O)C=1>C(O)C>[CH2:1]([N:3]([CH2:17][CH2:18][CH2:19][S:20]([CH2:21][CH2:22][CH3:23])=[O:31])[CH2:4][CH:5]([OH:16])[CH2:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([C:12]#[N:13])=[CH:14][CH:15]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 70297m-Chloroperbenzoic acidHCID 150668434-(3-{Ethyl[3-(propylsulfanyl)propyl]amino}-2-hydroxypropoxy)benzonitrile

生成物 1

HCID 3033962Almokalant

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
-10 °C

実験手順

2.45 g of 4-[3-[ethyl[3-(propylthio)propyl]amino]-2-hydroxypropoxy]-benzonitrile and 1.4 g p-toluenesulfonic acid were mixed in 50 ml of ethanol. The mixture was cooled to -10° C. and 1.7 g of m-chloroperbenzoic acid was added in small protions. The mixture was stirred for 0.5 hour at -10° C. and one hour at room temperature and then evaporated. The residue was dissolved in dichloromethane and washed with three portions of sodium carbonate and twice with water and thereafter dried over sodium sulfate, filtrated and evaporated. The residue, 2.3 g yellow oil, was purified by column chromatography. Yield: 1.4 g of the title compound.

後処理

  1. customevaporated
  2. dissolutionThe residue was dissolved in dichloromethane
  3. washwashed with three portions of sodium carbonate and twice with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltrated
  6. customevaporated
  7. customThe residue, 2.3 g yellow oil, was purified by column chromatography

出典と根拠

ORDレコード
ord-68d18174b05b400685f6a6fb7df98a6c
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05068272

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート