Water → 1-(2,5-Dichlorophenyl)-3-(1-methyl-2-pyrrolidylidene)urea

HRID 1973931

反応式

HRID 1973931 の反応式
Cl.[CH3:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[NH:8].O.[OH-].[Na+].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[N:20]=[C:21]=[O:22]>C1C=CC=CC=1>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[NH:20][C:21]([N:8]=[C:4]1[CH2:5][CH2:6][CH2:7][N:3]1[CH3:2])=[O:22]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 79360Benzene, 1,4-dichloro-2-isocyanato-HCID 124489671-Methylpyrrolidin-2-imine hydrochloride

生成物 1

HCID 542302811-(2,5-Dichlorophenyl)-3-(1-methyl-2-pyrrolidylidene)urea

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To 6.73 g. (0.05 mole) of 1-methyl-2-iminopyrrolidine HCl is added 1 ml. of water and 50 ml. of benzene. After solution is complete (magnetic stirring), 10 ml. of aqueous sodium hydroxide (50%) is added in one portion. After stirring for about 1 min., the benzene layer is decanted onto anhydrous potassium carbonate. The extraction is repeated twice. After drying (occasional swirling) the combined benzene extracts are filtered (dicalite) from drying agent and 9.4 g. (0.05 mole) of 2,5-dichlorophenylisocyanate is added to the filtrate in one portion with swirling. After stirring for 3 hours, the solvent is removed in vacuo affording a colorless solid 1-(2,5-dichlorophenyl)-3-(1-methyl-2-pyrrolidylidene)urea. Recrystallization from acetone (twice) yields the pure product, m.p. = 148.5°-150.5° C.

後処理

  1. stirringAfter stirring for about 1 min.
  2. customthe benzene layer is decanted onto anhydrous potassium carbonate
  3. extractionThe extraction
  4. dry with materialAfter drying (occasional swirling) the combined benzene extracts
  5. filtrationare filtered (dicalite)
  6. customfrom drying agent and 9.4 g
  7. stirringAfter stirring for 3 hours
  8. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-fb43956b0a6441b3af7a33f5128fb51d
出典データセット
uspto-grants-1976_12
特許番号
US03998958

関連ノート

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