Dimethylformamide dimethyl acetal → HCID 28887991、化合物

HRID 1988806ノート

反応式

HRID 1988806 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 28887991HCID 28887991、化合物収率 100.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c1ae9541110a4cd5b3bc31d9aa5cfb60
出典データセット
uspto-grants-2010_01
特許番号
US07642277B2

反応ノート

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