Hydroxide → Cymiazole

HRID 1679168ノート

反応式

HRID 1679168 の反応式
[C:1]1([NH:9][C:10]([NH:12][CH3:13])=[S:11])[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][C:2]=1[CH3:8].C(OC(O[CH2:21][CH3:22])CCl)C.[OH-]>Cl>[C:1]1([N:9]=[C:10]2[N:12]([CH3:13])[CH:22]=[CH:21][S:11]2)[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][C:2]=1[CH3:8]

参加物

5

反応物 3

HCID 961HydroxideHCID 121282-Chloro-1,1-diethoxyethaneHCID 30342141-(2,4-Dimethylphenyl)-3-methylthiourea

生成物 1

HCID 43714Cymiazole

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

19.4 g (0.1 mole) of N-2,4-xylyl-N'-methyl-thiourea and 15.2 g (0.1 mole) of chloroacetaldehyde-diethylacetal in 150 ml of 2N aqueous hydrochloric acid are refluxed for 1 hour. The clear light-yellow solution is subsequently cooled to room temperature; it is rendered slightly alkaline with 30% aqueous medium hydroxide solution, and extracted with ether. The ether extract is washed with water, dried with sodium sulphate and filtered, and the ether is then distilled off. The oily residue is distilled; b.p. 132°-134° C/0.3 Torr; yield: 20.2 g = 92% of theory.

後処理

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried with sodium sulphate
  5. filtrationfiltered
  6. distillationthe ether is then distilled off
  7. distillationThe oily residue is distilled

出典と根拠

ORDレコード
ord-17326f4df40341ea967ed5534a26a618
出典データセット
uspto-grants-1978_03
特許番号
US04079144

反応ノート

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