Trichloromethanesulfenyl chloride → HCID 18788458、化合物

HRID 442738ノート

反応式

HRID 442738 の反応式
[Cl:1][C:2](Cl)(Cl)[S:3]Cl.[CH3:7][C:8]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:9]=1[C:10]([NH2:12])=[NH:11].[OH-].[Na+]>ClCCl.O>[Cl:1][C:2]1[S:3][N:12]=[C:10]([C:9]2[C:8]([CH3:7])=[CH:16][C:15]([CH3:17])=[CH:14][C:13]=2[CH3:18])[N:11]=1

参加物

6

反応物 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 18788461Mesitylformamidin

生成物 1

HCID 18788458HCID 18788458、化合物収率 99.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

2.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After 1 hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.

後処理

  1. customthe precipitate formed
  2. customis isolated
  3. customthe organic phase is separated
  4. washwashed with 6 ml of water
  5. dry with materialAfter being dried over K2CO3, it
  6. concentrationis concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3347722aa6fb44c8b46f285d0212aaa5
出典データセット
uspto-grants-1999_04
特許番号
US05891894

反応ノート

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