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

HRID 544439

반응식

HRID 544439 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bef3c7e0cb9c46a391c6e7ccfbd4d97c
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04450169

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