Sodium benzenethiolate → 2-Chloro-3-phenylthio-6-nitro-N-methylaniline

HRID 1074848

반응식

HRID 1074848 반응식
[C:1]1([S-:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Na+].[Cl:9][C:10]1[C:17](Cl)=[CH:16][CH:15]=[C:14]([N+:19]([O-:21])=[O:20])[C:11]=1[NH:12][CH3:13]>C(#N)C>[Cl:9][C:10]1[C:17]([S:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:16][CH:15]=[C:14]([N+:19]([O-:21])=[O:20])[C:11]=1[NH:12][CH3:13]

참가 물질

4

반응물 2

HCID 4110039Sodium benzenethiolateHCID 204396362,3-dichloro-N-methyl-6-nitroaniline

생성물 1

HCID 204950262-Chloro-3-phenylthio-6-nitro-N-methylaniline

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

An amount of 2.9 gm of sodium thiophenolate was added to a solution of 4.4 gm (0.02 mol) of 2,3-dichloro-6-nitro-N-methylaniline dissolved in 50 ml of acetonitrile. The mixture was refluxed for half an hour and subsequently evaporated, and the residue was taken up with chloroform and water. The chloroform layer was separated, dried, and evaporated. Six grams of brown oil, which crystallized with isopropanol, were obtained. The yield from the crystallization was 4 gm of product (67.5% of theory) in the form of yellow crystals, m.p. 79° C.

후처리

  1. temperatureThe mixture was refluxed for half an hour
  2. customsubsequently evaporated
  3. customThe chloroform layer was separated
  4. customdried
  5. customevaporated
  6. customSix grams of brown oil, which crystallized with isopropanol
  7. customwere obtained
  8. customThe yield from the crystallization

출처 및 근거

ORD 기록
ord-f2d4cd2ada3d4c7b835e61681b1ae5d2
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04394159

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