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

HRID 27189
ノート
印刷プレビュー

反応式

HRID 27189 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine触媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-c00bccc821804a499ee7aafb396bbbca
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04220655

反応ノート

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