Benzene → 3-Chloromethyl-5-phenoxy-(1,2,4)-thiadiazole

HRID 544439

反応式

HRID 544439 の反応式
[CH:1]1[CH:6]=[CH:5][C:4]([O-:7])=[CH:3][CH:2]=1.[Na+].C1C=CC=CC=1.CN(C)C=O.[Cl:20][CH2:21][C:22]1[N:26]=[C:25](Cl)[S:24][N:23]=1>O>[Cl:20][CH2:21][C:22]1[N:26]=[C:25]([O:7][C:4]2[CH:5]=[CH:6][CH:1]=[CH:2][CH:3]=2)[S:24][N:23]=1

参加物

6

反応物 4

HCID 241BenzeneHCID 6228DimethylformamideHCID 3326105-Chloro-3-(chloromethyl)-1,2,4-thiadiazoleHCID 4445035Phenolate Sodium

生成物 1

HCID 131061443-Chloromethyl-5-phenoxy-(1,2,4)-thiadiazole収率 63.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5.8 g of sodium phenate were added to a mixture of 50 ml of benzene, 10 ml of dimethylformamide and 8.5 g of 3-chloromethyl-5-chloro-[1,2,4]-thiadiazole and the mixture was stirred at20° C. for 24 hours. 50 ml of water were added to the mixture and the decanted aqueous phase was extracted with benzene. The combined organic phase was dried and evaporated to dryness. The oil residue was distilled under reduced pressure to obtain 7.2 g of 3-chloromethyl-5-phenoxy-[1,2,4]-thiadiazole boiling at 114°-116° C. at 0.5 mm Hg.

後処理

  1. extractionthe decanted aqueous phase was extracted with benzene
  2. customThe combined organic phase was dried
  3. customevaporated to dryness
  4. distillationThe oil residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-bef3c7e0cb9c46a391c6e7ccfbd4d97c
出典データセット
uspto-grants-1984_05
特許番号
US04450169

関連ノート

読み込み中…