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Methanol → Difenzoquat metilsulfate

HRID 1457299
ノート
印刷プレビュー

反応式

HRID 1457299 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:5][C:4]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:3]1.[CH3:19]O.[S:21](=[O:25])(=[O:24])([OH:23])[OH:22]>ClCCCl>[CH3:19][O:24][S:21]([O-:23])(=[O:22])=[O:25].[CH3:1][N+:2]1[N:3]([CH3:19])[C:4]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:5][C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887Methanol2 回HCID 1118Sulfuric AcidHCID 1405171-Methyl-3,5-diphenylpyrazole

生成物 1

HCID 39424Difenzoquat metilsulfate収率 91.7%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
70 °C

実験手順

46.8 g (0.2 mol) of 1-methyl-3,5-diphenylpyrazole together with 40 g (1.25 mol) of methanol are introduced into the reaction vessel. After 19.4 g (0.19 mol) of 96% strength sulfuric acid have been added, the reaction solution is brought to 160° C. by distilling off methanol. 608 g (19 mol) of methanol are metered in below the surface of the reaction mixture in the course of 7.5 hours. After the mixture has been cooled to 70° C., 25 g of 1,2-dichloroethane are added, and the mixture is cooled to room temperature with stirring. The reaction mixture is filtered and washed with 12.5 g of 1,2-dichloroethane. 67.7 g of 1,2-dimethyl-3,5-diphenylpyrazolium methylsulfate with a content of 97.5% (HPLC) of m.p. 157°-159° C. are obtained, which corresponds to a yield of 91.7% of theory.

後処理

  1. customis brought to 160° C.
  2. distillationby distilling off methanol
  3. customare metered in below the surface of the reaction mixture in the course of 7.5 hours
  4. temperaturethe mixture is cooled to room temperature
  5. filtrationThe reaction mixture is filtered
  6. washwashed with 12.5 g of 1,2-dichloroethane

出典と根拠

ORDレコード
ord-5622c04bb79143c7bf771a1e6edfa8d4
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05847154

反応ノート

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