Benzenesulfenyl chloride → 1-Methyl-2-[nitro(phenylsulfanyl)methylidene]imidazolidine

HRID 1973248노트

반응식

HRID 1973248 반응식
[C:1]1([S:7]Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:9][N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[CH:15][N+:16]([O-:18])=[O:17]>N1C=CC=CC=1>[CH3:9][N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[C:15]([N+:16]([O-:18])=[O:17])[S:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 11008040Benzenesulfenyl chlorideHCID 702500461-Methyl-2-(nitromethylidene)imidazolidine

생성물 1

HCID 706390091-Methyl-2-[nitro(phenylsulfanyl)methylidene]imidazolidine

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

14.6 g of phenylsulfenyl chloride was added dropwise to a cooled, stirred solution of 14.3 g of Compound 1A in 250 ml of pyridine. The mixture was allowed to stand overnight at room temperature, then excess pyridine was recovered on a rotary evaporator. The residue was treated with 250 ml of water and the mixture was extracted with methylene chloride. The combined extracts were dried and the solvent was evaporated to give a crystalline solid which was triturated with ethyl acetate, then ethanol, to yield 1-methyl-2-(nitro(phenylthio)methylene)imidazolidine (1B) as a yellow solid, melting point: 170°-173°.

후처리

  1. customexcess pyridine was recovered on a rotary evaporator
  2. additionThe residue was treated with 250 ml of water
  3. extractionthe mixture was extracted with methylene chloride
  4. customThe combined extracts were dried
  5. customthe solvent was evaporated
  6. customto give a crystalline solid which
  7. customwas triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-10851a51b61841f68b7df67583548852
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996372

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