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O-Xylene → 3,4-Dimethylbenzene-1-carbothioamide

HRID 436310
ノート
印刷プレビュー

反応式

HRID 436310 の反応式
[S-:1][C:2]#[N:3].[K+].[CH3:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=1[CH3:12].F>>[CH3:5][C:6]1[CH:7]=[C:8]([CH:9]=[CH:10][C:11]=1[CH3:12])[C:2]([NH2:3])=[S:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 7237O-XyleneHCID 14917Hydrofluoric AcidHCID 516872Potassium thiocyanate

生成物 1

HCID 204708513,4-Dimethylbenzene-1-carbothioamide

実験手順

At a temperature as indicated in Example 1, 59 g of potassium thiocyanate (0.6 mol) and 79.5 g of o-xylene (0.75 mol) are stirred with 0.5 l of 98% hydrofluoric acid. and the mixture is then stirred for 10 hours at room temperature. Subsequently, the batch is poured onto ice, the precipitated product is suction-filtered after having been stirred for one-half hour, and the greater part of the non-reacted o-xylene (15 g) is separated from the still moist filter cake by steam distillation. The distillation residue is subsequently suction-filtered and dried. The yield of dimethylthiobenzamide having a melting point of 120° - 125° C is 99 g and therefore quantitative, relative to the potassium thiocyanate used.

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  • additionSubsequently, the batch is poured onto ice
  • filtrationthe precipitated product is suction-filtered
  • stirringafter having been stirred for one-half hour
  • customthe greater part of the non-reacted o-xylene (15 g) is separated from the still moist filter cake by steam distillation
  • filtrationThe distillation residue is subsequently suction-filtered
  • customdried
  • 出典と根拠

    ORDレコード
    ord-97dcba008f2441af99e13f908a27b9ec
    出典データセット
    uspto-grants-1977_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04008264

    反応ノート

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