Acetic Acid → HCID 365395、化合物

HRID 2083437ノート

反応式

HRID 2083437 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 365395HCID 365395、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-382552836f3e47128d49ecf4f8faba08
出典データセット
uspto-grants-1978_04
特許番号
US04085273

反応ノート

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