3-Chloroaniline → 3-((3-Chlorophenyl)amino)-2-cyano-3-(methylthio)acrylamide

HRID 527273

反応式

HRID 527273 の反応式
[C:1]([C:3](=[C:7]([S:10][CH3:11])SC)[C:4]([NH2:6])=[O:5])#[N:2].[Cl:12][C:13]1[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=1)[NH2:16]>C(O)C>[Cl:12][C:13]1[CH:14]=[C:15]([NH:16][C:7]([S:10][CH3:11])=[C:3]([C:1]#[N:2])[C:4]([NH2:6])=[O:5])[CH:17]=[CH:18][CH:19]=1

参加物

4

実験手順

Dissolved 7.00 g (2-cyano-3,3-bis(methylthio)acrylamide) in 125 mL of ethanol. Then added 4.348 mL (1.10 eq.) of 3-chloroaniline to the reaction vessel and stirred the reaction at 75° C. until starting amide was absent and confirmed by HPLC. Once complete (18 hrs), the reaction was brought to room temperature and filtered to obtain 3-((3-chlorophenyl)amino)-2-cyano-3-(methylthio)acrylamide as an off white to light yellow powder. Product was allowed to dry under vacuum for 1 hr (6.0 g, 57% yield).

後処理

  1. customthe reaction at 75° C.
  2. customOnce complete (18 hrs)
  3. customwas brought to room temperature
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-13c5edb632ed4d19a0e351cf17c50515
出典データセット
uspto-grants-2016_05
特許番号
US09346792B2

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