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Acetone → 3-(2-Chlorobenzoyl)-2-(2-nitroethenylamino)-5-ethylthiophene

HRID 1657225
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HRID 1657225 반응식
[NH2:1][C:2]1[S:3][C:4]([CH2:16][CH3:17])=[CH:5][C:6]=1[C:7](=[O:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:14].O1CCN([CH:24]=[CH:25][N+:26]([O-:28])=[O:27])CC1.Cl.CC(C)=O>O>[Cl:14][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[C:7]([C:6]1[CH:5]=[C:4]([CH2:16][CH3:17])[S:3][C:2]=1[NH:1][CH:24]=[CH:25][N+:26]([O-:28])=[O:27])=[O:15]
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참가 물질

6

반응물 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 683970Morpholine, 4-(2-nitroethenyl)-HCID 13163365(2-Amino-5-ethylthiophen-3-yl)(2-chlorophenyl)methanone

생성물 1

HCID 677573983-(2-Chlorobenzoyl)-2-(2-nitroethenylamino)-5-ethylthiophene수율 84.1%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

A mixture of 2-amino-3-(2-chlorobenzoyl)-5-ethylthiophene (5.30 g), 1-morpholino-2-nitroethene (3.16 g), 6N HCl (5 ml) and acetone (25 ml) was stirred at room temperature for one hour. Water was added to the mixture, which was extracted with ethene acetate. The extract was washed with water and dried over MgSO4, and then the solvent was distilled off to obtain 3-(2-chlorobenzoyl)-2-(2-nitroethenylamino)-5-ethylthiophene as crystals (5.65 g, 84.1%). The crystals were recrystallized from acetone to obtain yellow plates, mp: 125°-126° C.

후처리

  1. extractionwas extracted with ethene acetate
  2. washThe extract was washed with water
  3. dry with materialdried over MgSO4
  4. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-cf6260d2376e4a2f9682a1bf93b9c72e
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05256782

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