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

HRID 2412926ノート

反応式

HRID 2412926 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 13370531HCID 13370531、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b63dc983b38846d48f43eeaf6bfffb1c
出典データセット
uspto-grants-1985_01
特許番号
US04495195

反応ノート

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