Ethanol → 1-(Ethoxycarbonyl)ethyl 4-[13-(4-chlorophenyl)tridec-12-ynylamino]benzoate

HRID 2057666ノート

反応式

HRID 2057666 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][C:22]2[CH:30]=[CH:29][C:25]([C:26]([O-:28])=[O:27])=[CH:24][CH:23]=2)=[CH:4][CH:3]=1.[Na+].C(O)C.S(O[CH:46]([CH3:52])[C:47]([O:49][CH2:50][CH3:51])=[O:48])(C1C=CC(C)=CC=1)(=O)=O>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][C:22]2[CH:23]=[CH:24][C:25]([C:26]([O:28][CH:46]([C:47]([O:49][CH2:50][CH3:51])=[O:48])[CH3:52])=[O:27])=[CH:29][CH:30]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 702EthanolHCID 562846Ethyl 2-[(4-methylbenzenesulfonyl)oxy]propanoateHCID 23706318Sodium 4-[13-(4-chlorophenyl)tridec-12-ynylamino]benzoate

生成物 1

HCID 203313231-(Ethoxycarbonyl)ethyl 4-[13-(4-chlorophenyl)tridec-12-ynylamino]benzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a warm mixture of 7 g. sodium 4-[13-(4-chlorophenyl)tridec-12-ynylamino]benzoate in 100 ml. ethanol is added 4.7 g. ethyl α-tosyloxypropionate. After 17 hours at reflux, the cooled solution is diluted with an equal volume of water and the resultant precipitate is filtered. After washing with cold ethanol and drying, the product is crystallized from acetonitrile to yield 1-(ethoxycarbonyl)ethyl 4-[13-(4-chlorophenyl)tridec-12-ynylamino]benzoate as colorless crystals.

後処理

  1. additionTo a warm mixture of 7 g
  2. temperatureAfter 17 hours at reflux
  3. filtrationthe resultant precipitate is filtered
  4. washAfter washing with cold ethanol
  5. customdrying
  6. customthe product is crystallized from acetonitrile

出典と根拠

ORDレコード
ord-f8dd1fe34fb64234a6cf629a03d116fc
出典データセット
uspto-grants-1980_07
特許番号
US04211783

反応ノート

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