Dichloromethane → HCID 13799792, 화합물

HRID 1906395노트

반응식

HRID 1906395 반응식
[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]

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 13799782HCID 13799782, 화합물2회HCID 20211738Tetrachloroethylsulfenyl chloride

생성물 1

HCID 13799792HCID 13799792, 화합물

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2d4d96b7de5843a2be97d7e55488460c
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04652556

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