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Potassium Carbonate → 2-Methylimino-3-methyl-5-benzyl-tetrahydro-1,3,5-thiadiazin-4-one

HRID 237074
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반응식

HRID 237074 반응식
[CH2:1]([N:8]([CH2:12]Cl)[C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:14][NH:15][C:16]([NH:18][CH3:19])=[S:17].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:14][N:15]=[C:16]1[N:18]([CH3:19])[C:9](=[O:10])[N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:12][S:17]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2723631N,N'-DimethylthioureaHCID 21314706N-benzyl-N-chloromethylcarbamoyl chloride

생성물 1

HCID 213147022-Methylimino-3-methyl-5-benzyl-tetrahydro-1,3,5-thiadiazin-4-one수율 80.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4.4 g (0.02 mole) of N-benzyl-N-chloromethylcarbamoyl chloride and 2.0 g (0.02 mole) of 1,3-dimethylthiourea was dissolved in 50 ml of ethyl alcohol and heated under reflux with stirring for 2 hours. After addition of 20 ml of a saturated aqueous potassium carbonate solution, the mixture was extracted with 100 ml of benzene. The benzene layer was washed with water, dried, and freed from the benzene by distillation under reduced pressure to obtain 4.0 g of crude crystals which were recrystallized from ether. Yield 3.2 g (63%); m.p. 93°-95° C.

후처리

  1. temperatureheated
  2. temperatureunder reflux
  3. extractionthe mixture was extracted with 100 ml of benzene
  4. washThe benzene layer was washed with water
  5. customdried
  6. distillationfreed from the benzene by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-7ce92d3519144c1d8a85ec3ce9a8d49e
출처 데이터셋
uspto-grants-1979_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04159328

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