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

HRID 1973931

반응식

HRID 1973931 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fb43956b0a6441b3af7a33f5128fb51d
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998958

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