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

HRID 2057666노트

반응식

HRID 2057666 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f8dd1fe34fb64234a6cf629a03d116fc
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04211783

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