Water → Methyl 1-methyl-3-(3-bromophenyl)-4-chloropyrazole-5-carboxylate

HRID 2412926노트

반응식

HRID 2412926 반응식
[CH3:1][N:2]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Br:17])[CH:12]=2)=[N:3]1.S(Cl)([Cl:21])(=O)=O.O>C1C=CC=CC=1>[CH3:1][N:2]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[C:5]([Cl:21])[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Br:17])[CH:12]=2)=[N:3]1

참가 물질

5

반응물 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 13370531HCID 13370531, 화합물

생성물 1

HCID 13370534Methyl 1-methyl-3-(3-bromophenyl)-4-chloropyrazole-5-carboxylate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A reaction mixture was prepared from 13.5 g. of methyl 1-methyl-3-(3-bromophenyl)pyrazole-5-carboxylate and 6.2 g. of sulfuryl chloride in benzene solution. The reaction mixture was heated to refluxing temperature for about 36 hours, and was then cooled and poured into water. The aqueous mixture was extracted with ethyl acetate, and the ethyl acetate extract separated and dried. Removal of the ethyl acetate in vacuo yielded, as a residue, methyl 1-methyl-3-(3-bromophenyl)-4-chloropyrazole-5-carboxylate formed in the above reaction. Recrystallization of the residue from hexane yielded crystalline material melting at 91°-3° C.

후처리

  1. customA reaction mixture was prepared from 13.5 g
  2. temperatureThe reaction mixture was heated
  3. temperatureto refluxing temperature for about 36 hours
  4. temperaturewas then cooled
  5. extractionThe aqueous mixture was extracted with ethyl acetate
  6. extractionthe ethyl acetate extract
  7. customseparated
  8. customdried
  9. customRemoval of the ethyl acetate in vacuo
  10. customyielded, as a residue

출처 및 근거

ORD 기록
ord-b63dc983b38846d48f43eeaf6bfffb1c
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04495195

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