Ethanethiol → 2-Chloro-1-[3-(ethyldisulfanyl)-4-nitrophenoxy]-4-(trifluoromethyl)benzene

HRID 485619노트

반응식

HRID 485619 반응식
[CH2:1]([SH:3])[CH3:2].C(N(CC)CC)C.[Cl:11][C:12]1[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:27]=[CH:26][C:13]=1[O:14][C:15]1[CH:16]=[C:17]([S:24]Cl)[C:18]([N+:21]([O-:23])=[O:22])=[CH:19][CH:20]=1>CCOCC>[CH2:1]([S:3][S:24][C:17]1[C:18]([N+:21]([O-:23])=[O:22])=[CH:19][CH:20]=[C:15]([O:14][C:13]2[CH:26]=[CH:27][C:28]([C:30]([F:31])([F:32])[F:33])=[CH:29][C:12]=2[Cl:11])[CH:16]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 6343EthanethiolHCID 8471TriethylamineHCID 13246608HCID 13246608, 화합물

생성물 1

HCID 132466102-Chloro-1-[3-(ethyldisulfanyl)-4-nitrophenoxy]-4-(trifluoromethyl)benzene수율 98%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

1.62 parts by weight of ethanethiol and 2.6 parts by weight of triethylamine were added simultaneously to a solution of 10 parts by weight of 3-(2'-chloro-4'-trifluoromethylphenoxy)-6-nitrobenzenesulfenyl chloride in 100 parts by volume of absolute ether, and stirring was continued for a further 2 hours at room temperature. The reaction mixture was filtered, and the filtrate was extracted with dilute aqueous hydrochloric acid and water, dried over magnesium sulfate, filtered, and evaporated down under reduced pressure. 8 parts by weight (98% yield) of 3-(2'-chloro-4'-trifluoromethylphenoxy)-6-nitrophenyl ethyl disulfide of refractive index nD25 : 1.6067 were obtained (compound No. 4).

후처리

  1. filtrationThe reaction mixture was filtered
  2. extractionthe filtrate was extracted with dilute aqueous hydrochloric acid and water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated down under reduced pressure

출처 및 근거

ORD 기록
ord-ca61ce8ca4cc42738951e2ec4ebfa32e
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04537621

반응 노트

불러오는 중…