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

HRID 485619ノート

反応式

HRID 485619 の反応式
[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]

参加物

5

反応物 3

HCID 6343EthanethiolHCID 8471TriethylamineHCID 13246608HCID 13246608、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ca61ce8ca4cc42738951e2ec4ebfa32e
出典データセット
uspto-grants-1985_08
特許番号
US04537621

反応ノート

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