Dichloromethane → 5-Chloro-3-(4-nitrophenyl)-1,2,4-thiadiazole

HRID 236650

反応式

HRID 236650 の反応式
[OH-].[Na+].Cl.[N+:4]([C:7]1[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=[NH:12])=[CH:9][CH:8]=1)([O-:6])=[O:5].[Cl:16][C:17]([SH:20])(Cl)Cl.ClCCl>O>[Cl:16][C:17]1[S:20][N:13]=[C:11]([C:10]2[CH:9]=[CH:8][C:7]([N+:4]([O-:6])=[O:5])=[CH:15][CH:14]=2)[N:12]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 6390TrichloromethanethiolHCID 14798Sodium HydroxideHCID 1706254-Nitrobenzamidine hydrochloride

生成物 1

HCID 202163765-Chloro-3-(4-nitrophenyl)-1,2,4-thiadiazole収率 40.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 75.6 gm of sodium hydroxide in 100 ml of water was added to a stirred mixture of 101.4 gm of p-nitrobenzamidine hydrochloride, 70 gm of perchloromethyl mercaptan and 760 ml of dichloromethane, while keeping the temperature below -5° C. After additional 2 hours at -5° C., the resulting suspension was filtered, and the organic phase was separated, evaporated to dryness, and the residual solid was recrystallized from 95% ethanol, yielding 45 gm of the title compound, m.p. 143°-145° C.

後処理

  1. customthe temperature below -5° C
  2. filtrationthe resulting suspension was filtered
  3. customthe organic phase was separated
  4. customevaporated to dryness
  5. customthe residual solid was recrystallized from 95% ethanol

出典と根拠

ORDレコード
ord-8c605c6e3cf44e91b096dd9b2dbdd058
出典データセット
uspto-grants-1987_02
特許番号
US04645841

関連ノート

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