HCID 23053854、化合物 → HCID 13649684、化合物

HRID 280659ノート

反応式

HRID 280659 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Cl:12])[C:10]=1Cl)[C:5]([NH2:7])=[O:6].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([S-:20])=[CH:16][CH:15]=1.[K+]>CN(C)C=O>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([S:20][C:10]2[C:9]([Cl:12])=[CH:8][C:4]([C:5]([NH2:7])=[O:6])=[CH:3][C:2]=2[Cl:1])=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 23053854HCID 23053854、化合物HCID 23693160HCID 23693160、化合物

生成物 1

HCID 13649684HCID 13649684、化合物収率 57.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3,4,5-trichlorobenzamide (25.0 g, 111 mmol) and potassium 4-chlorothiophenolate (29.0 g, 159 mmol) in dimethylformamide (220 ml) was stirred for 3 days at ambient temperature under nitrogen atmosphere, poured into ice water (2.2 L), and filtered. The solid was washed with water, partially dried under vacuum, suspended in diethyl ether (200 ml), filtered, and washed with diethyl ether (2×75 ml). The residue was triturated with diethyl ether (75 ml), filtered, again triturated with diethyl ether (75 ml), filtered, and dried under vacuum to provide 21.2 g (57%) of 4-(4-chlorophenylthio)-3,5-dichlorobenzamide, m.p. 171°-174° C.

後処理

  1. filtrationfiltered
  2. washThe solid was washed with water
  3. custompartially dried under vacuum
  4. filtrationfiltered
  5. washwashed with diethyl ether (2×75 ml)
  6. customThe residue was triturated with diethyl ether (75 ml)
  7. filtrationfiltered
  8. customagain triturated with diethyl ether (75 ml)
  9. filtrationfiltered
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-5b10938079df4a19a660590971585767
出典データセット
uspto-grants-1986_05
特許番号
US04590201

反応ノート

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