Hydroxide → Cymiazole

HRID 1679168노트

반응식

HRID 1679168 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 43714Cymiazole

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-17326f4df40341ea967ed5534a26a618
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04079144

반응 노트

불러오는 중…