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Hexane → HCID 178470096, 화합물

HRID 1722071
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HRID 1722071 반응식
[F:1][C:2]1[C:30]([F:31])=[C:29]([F:32])[CH:28]=[CH:27][C:3]=1[NH:4][C:5](=[C:16]([C:22](OCC)=[O:23])[C:17]([O:19][CH2:20][CH3:21])=[O:18])[S:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1.CCCCCC>C1(OC2C=CC=CC=2)C=CC=CC=1>[OH:23][C:22]1[C:27]2[C:3](=[C:2]([F:1])[C:30]([F:31])=[C:29]([F:32])[CH:28]=2)[N:4]=[C:5]([S:6][CH2:7][C:8]2[CH:9]=[CH:10][C:11]([O:14][CH3:15])=[CH:12][CH:13]=2)[C:16]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8058HexaneHCID 14673304Diethyl [(2,3,4-trifluoroanilino)(p-methoxybenzylthio)methylene]malonate

생성물 1

HCID 178470096HCID 178470096, 화합물수율 82.1%

시약·촉매·용매 1

HCID 7583Diphenyl Ether용매2회

실험 절차

A solution of diethyl [(2,3,4-trifluoroanilino)(p-methoxybenzylthio)methylene]malonate (80.9 g) in diphenyl ether (60 ml) heated at 110° C. was added dropwise to diphenyl ether (210 ml) kept at 250° to 260° C. with stirring under nitrogen stream over a period of 15 minutes. After the reaction mixture was further stirred at the same temperature for 5 minutes, the mixture was cooled to room temperature and added to hexane (3000 ml). The resulting precipitate was filtered to give the title compound (59.9 g), which was recrystallized from ethyl acetate to give yellow crystals, m.p. 174°-176° C.

후처리

  1. customkept at 250° to 260° C.
  2. stirringAfter the reaction mixture was further stirred at the same temperature for 5 minutes
  3. filtrationThe resulting precipitate was filtered

출처 및 근거

ORD 기록
ord-28d48a26bce1447c8d43b1789585e0bc
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04853469

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