HCID 23053854, 화합물 → HCID 13649684, 화합물

HRID 280659노트

반응식

HRID 280659 반응식
[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

참가 물질

4

반응물 2

HCID 23053854HCID 23053854, 화합물HCID 23693160HCID 23693160, 화합물

생성물 1

HCID 13649684HCID 13649684, 화합물수율 57.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b10938079df4a19a660590971585767
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04590201

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