Acetic Acid → HCID 365395, 화합물

HRID 1973771노트

반응식

HRID 1973771 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]Cl)=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[C:13](O)(=O)[CH3:14]>C(OCC)C>[N+:10]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[S:8][C:14]1[CH:13]=[CH:7][C:2]([Cl:1])=[CH:3][C:4]=1[N+:10]([O-:12])=[O:11])([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 10443590Benzenesulfenyl chloride, 4-chloro-2-nitro-

생성물 1

HCID 365395HCID 365395, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To 1.37 g. of 3-butenyltributyltin was added 0.89 g. of 4-chloro-2-nitrobenzene sulfenyl chloride dissolved in 20 ml. glacial acetic acid at steam bath temperature. The mixture was then heated on a steam bath for 30 minutes and poured into an ice water bath. The product was taken up in diethyl ether, washed twice with 50 ml. portions of water, twice with 50 ml. portions of saturated sodium bicarbonate and an additional time with 50 ml. of water. The resulting ether layer was separated, dried over magnesium sulfate and filtered. The solvent was removed on a rotary evaporator and the concentrate analyzed by proton nmr. The product proved to be cyclopropylcarbinyl 2-nitro-4-chlorophenyl sulfide.

후처리

  1. temperatureThe mixture was then heated on a steam bath for 30 minutes
  2. additionpoured into an ice water bath
  3. washwashed twice with 50 ml
  4. customThe resulting ether layer was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customThe solvent was removed on a rotary evaporator

출처 및 근거

ORD 기록
ord-c85c1ce5f4434455b0a5a5e4c024c2f8
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998889

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