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Water → HCID 178503870, 화합물

HRID 1578043
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HRID 1578043 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]([NH:12][C:13](=[O:15])[CH3:14])=[S:11].[C:16]([O-])([O-])=O.[K+].[K+].O.CI>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10](=[N:12][C:13](=[O:15])[CH3:14])[S:11][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 12952276HCID 12952276, 화합물

생성물 1

HCID 178503870HCID 178503870, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

26.3 g (0.1M) of N-(2,6-dichlorophenyl)-N'-acetylthiourea, 9.9 g (0.06M) of ground 2 K2CO3.3 H2O, 8.3 ml (0.13M) of methyliodide and 200 ml of acetone are put to boil and are energetically shaken for 5 hours. The acetone is distilled off and the residue is washed with water and filtered. The sediment on the filter is washed once or twice more with water. After drying the product is boiled in a reflux with isopropanol 1:6, weight:volume) and is filtered. From the filtrate 22.0 g of N-(2,6-dichloro-phenyl)-N'-acetyl-S-methylisothiourea (79.4% of the theoretical yield), melting point 137° to 140° C. are isolated.

후처리

  1. distillationThe acetone is distilled off
  2. washthe residue is washed with water
  3. filtrationfiltered
  4. washThe sediment on the filter is washed once or twice more with water
  5. customAfter drying the product
  6. temperaturea reflux with isopropanol 1:6, weight
  7. filtrationvolume) and is filtered

출처 및 근거

ORD 기록
ord-b66265b799d3498aab15003784387e88
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04290971

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