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1,2-Dimethoxyethane → N-(3',4'-Dichlorophenyl)-3,4-dimethyl-2-methyl-carbamoyloxy-5-oxo-2,5-dihydropyrrole

HRID 1390170
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HRID 1390170 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]2[OH:17])[CH:5]=[CH:6][C:7]=1[Cl:8].C[N:19]=[C:20]=[O:21].[CH3:22]OCCOC>C(N(CC)CC)C>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:10](=[O:17])[C:11]([CH3:16])=[C:12]([CH3:15])[C:13]2([O:14][C:20](=[O:21])[NH2:19])[CH3:22])[CH:5]=[CH:6][C:7]=1[Cl:8]
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참가 물질

5

반응물 3

HCID 80711,2-DimethoxyethaneHCID 12228Methyl IsocyanateHCID 13069714N-(3',4'-Dichlorophenyl)-3,4-dimethyl-2-hydroxy-5-oxo-2,5-dihydropyrrole

생성물 1

HCID 86736277N-(3',4'-Dichlorophenyl)-3,4-dimethyl-2-methyl-carbamoyloxy-5-oxo-2,5-dihydropyrrole

시약·촉매·용매 1

HCID 8471Triethylamine촉매

실험 절차

16.3 g of N-(3',4'-dichlorophenyl)-3,4-dimethyl-2-hydroxy-5-oxo-2,5-dihydropyrrole (see Example 3) is put together with 2 drops of triethylamine in 10 ml of glyme (ethylene glycol dimethyl ether), and 3.8 g of methylisocyanate is then added. After 24 hours, the reaction solution is filtered with a filtering auxiliary (Hyflo®) and the filtrate is concentrated by evaporation to leave an oil, which is crystallised in methanol. In this manner is obtained 15 g (76% of theory) of the above product in the form of yellowish crystals, m.p. 141°-142°.

후처리

  1. additionis then added
  2. filtrationthe reaction solution is filtered with a filtering auxiliary (Hyflo®)
  3. concentrationthe filtrate is concentrated by evaporation
  4. customto leave an oil, which
  5. customis crystallised in methanol
  6. customIn this manner is obtained 15 g (76% of theory) of the above product in the form of yellowish crystals, m.p. 141°-142°

출처 및 근거

ORD 기록
ord-24107451a5a04980b503140abfbf9ea9
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04138243

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