Sulfuric Acid → 1-Bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene

HRID 2380205

반응식

HRID 2380205 반응식
[OH-].C([N+](C)(C)C)C1C=CC=CC=1.[Br:13][C:14](Br)=[CH:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH3:23])=[CH:18][C:17]=1[Cl:24].S(=O)(=O)(O)O>CO.C1(C)C=CC=CC=1>[Br:13][C:14]#[C:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH3:23])=[CH:18][C:17]=1[Cl:24]

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 66854Benzyltrimethylammonium hydroxideHCID 199317831,1-Dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene

생성물 1

HCID 199317681-Bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene수율 12,381.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매2회

실험 절차

A suspension of Triton B (Reg Trade Mark, N-benzyltrimethylammonium hydroxide, 40% in methanol, 1.8 g) in toluene was added to a solution of 1,1-dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene (0.96 g) in toluene. The mixture was stirred for 15 minutes. Sulphuric acid (2 m) was added and the resulting layers were separated. The organic layer was washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromotography eluted with a mixture of hexane and dichloromethane to give 1-bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene 90.78 g) as a yellow oil, NMR (CDCl3) 2.5 (s,3H), 7.05(d,1H), 7.2(s,1H), 7.35(d,1H).

후처리

  1. customthe resulting layers were separated
  2. washThe organic layer was washed with water
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness
  6. customthe residue was purified by chromotography
  7. washeluted with a mixture of hexane and dichloromethane

출처 및 근거

ORD 기록
ord-b0fc333b1103453e919e5952f75d304f
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05366957

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