Water → Xilobam

HRID 1973930노트

반응식

HRID 1973930 반응식
Cl.[CH3:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[NH:8].O.[OH-].[Na+].[CH3:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[C:14]=1[N:20]=[C:21]=[O:22]>C1C=CC=CC=1>[CH3:19][C:15]1[CH:16]=[CH:17][CH:18]=[C:13]([CH3:12])[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 987872,6-Xylyl isocyanateHCID 124489671-Methylpyrrolidin-2-imine hydrochloride

생성물 1

HCID 39689Xilobam

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a stirring solution of 6.73 g. (0.05 mole) of 1-methyl- 2-iminopyrrolidine hydrochloride in about 2 ml. of water is added about 50 ml. of benzene followed by 10 ml. of 50% NaOH. After stirring 1 min. the benzene layer is decanted onto anhydrous potassium carbonate. The extraction is repeated twice. The combined benzene extracts are filtered from a drying agent (dicalite pad) and rinsed well with dry benzene. To the filtrate is added in one portion with stirring 7.36 g. (0.05 mole) of 2,6-dimethylphenylisocyanate. The reaction mixture is stirred overnight. Solvent removal and recrystallization from ethyl acetate-ether gives the product, 1-(2,6 -dimethylphenyl)-3-(1-methyl-2-pyrrolidylidene)urea, as white crystals, m.p. = 119°-120° C.

후처리

  1. customis decanted onto anhydrous potassium carbonate
  2. extractionThe extraction
  3. filtrationThe combined benzene extracts are filtered from a drying agent (dicalite pad)
  4. washrinsed well with dry benzene
  5. additionTo the filtrate is added in one portion
  6. stirringThe reaction mixture is stirred overnight
  7. customSolvent removal and recrystallization from ethyl acetate-ether

출처 및 근거

ORD 기록
ord-c9c45004406b44bfbb0dfc6151186571
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998958

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