Dichloromethane → HCID 13799792、化合物

HRID 1906395ノート

反応式

HRID 1906395 の反応式
[CH3:1][C:2]([NH:6][S:7]([CH2:10][CH2:11][CH2:12][Cl:13])(=[O:9])=[O:8])([CH3:5])[C:3]#[N:4].[Cl:14][CH:15]([S:20]Cl)[C:16](Cl)([Cl:18])[Cl:17].[OH-].[Na+].C(Cl)[Cl:25]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.O>[Cl:25][C:15]([Cl:14])([S:20][N:6]([C:2]([C:3]#[N:4])([CH3:1])[CH3:5])[S:7]([CH2:10][CH2:11][CH2:12][Cl:13])(=[O:8])=[O:9])[CH:16]([Cl:18])[Cl:17]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 13799782HCID 13799782、化合物2 回HCID 20211738Tetrachloroethylsulfenyl chloride

生成物 1

HCID 13799792HCID 13799792、化合物

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒HCID 962Water溶媒

実験手順

To a stirred mixture of 2.25 g (0.01 mole) 2-methyl-2-(3-chloropropylsulfonamido)propionitrile (the product of Example 35) and 2.87 g (0.011 mole) tetrachloroethylsulfenyl chloride with 0.1 g benzyltriethylammonium chloride in 100 ml methylene chloride, 0.48 g [(0.012 mole) 0.96 g as a 50% weight/weight solution] sodium hydroxide dissolved in 20 ml water was added slowly. The reaction mixture was stirred for three hours. The mixture was washed three times with 100 ml water. The organic layers were dried over calcium sulfate and evaporated to give a dark brown oil which crystallized upon standing overnight. The crystals were washed with hexane to give the above-identified product, as a brown solid, melting point 68°-71° C.

後処理

  1. additionwas added slowly
  2. washThe mixture was washed three times with 100 ml water
  3. dry with materialThe organic layers were dried over calcium sulfate
  4. customevaporated
  5. customto give a dark brown oil which
  6. customcrystallized
  7. waitupon standing overnight
  8. washThe crystals were washed with hexane
  9. customto give the above-identified product

出典と根拠

ORDレコード
ord-2d4d96b7de5843a2be97d7e55488460c
出典データセット
uspto-grants-1987_03
特許番号
US04652556

反応ノート

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