Dimethylformamide dimethyl acetal → HCID 28887991, 화합물

HRID 1988806노트

반응식

HRID 1988806 반응식
[C:1]1([NH:11][C:12](=[S:15])[NH:13][NH2:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[CH3:16]OC(OC)N(C)C>O1CCOCC1>[C:1]1([N:11]2[CH:16]=[N:14][NH:13][C:12]2=[S:15])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 2760175N-(Naphthalen-1-yl)hydrazinecarbothioamide

생성물 1

HCID 28887991HCID 28887991, 화합물수율 100.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 4-(1-naphthalenyl)-3-thiosemicarbazide (4.01 g, 18.4 mmol) and N,N,-dimethylformamide dimethyl acetal (2.50 mL, 18.8 mmol) in 1,4-dioxane (40 mL) was stirred at room temperature for 16 h. The mixture was concentrated under reduced pressure. The residue was taken in hexane and Et2O and the solution was stirred until a suspension was obtained. The suspension was filtered and the solid was triturated with hexane:Et2O (4:1), then was dried under reduced pressure to give the title compound (4.19 g, 90% yield) as a beige solid.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customwas obtained
  3. filtrationThe suspension was filtered
  4. customthe solid was triturated with hexane:Et2O (4:1)
  5. customwas dried under reduced pressure

출처 및 근거

ORD 기록
ord-c1ae9541110a4cd5b3bc31d9aa5cfb60
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642277B2

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