Tetrafluoroborate → 1-(1-Benzyl-2-pyrrolidylidene)-3-(2,6-dimethylphenyl)urea

HRID 1973941

반응식

HRID 1973941 반응식
F[B-](F)(F)F.[CH2:6]([N:13]1[CH2:17][CH2:16][CH2:15][C:14]1=[NH:18])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[CH3:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1[N:27]=[C:28]=[O:29]>>[CH2:6]([N:13]1[CH2:17][CH2:16][CH2:15][C:14]1=[N:18][C:28]([NH:27][C:21]1[C:20]([CH3:19])=[CH:25][CH:24]=[CH:23][C:22]=1[CH3:26])=[O:29])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

4

반응물 3

HCID 26255TetrafluoroborateHCID 987872,6-Xylyl isocyanateHCID 124490231-Benzyl-2-iminopyrrolidine

생성물 1

HCID 543734621-(1-Benzyl-2-pyrrolidylidene)-3-(2,6-dimethylphenyl)urea

실험 절차

The fluoroborate salt of 1-benzyl-2-iminopyrrolidine (6.55 g.; 0.025 mole) is converted to free base (4.36 g.; 0.025 mole) in the usual manner. After drying over K2CO3, the benzene solution is filtered through diatomaceous earth and 3.68 g. (0.025 mole) of 2,6-dimethylphenylisocyanate is added. The reaction mixture is stirred at room temperature for 1 hour and then evaporated to dryness in vacuo to give an oily residue of 1-(1-benzyl-2-pyrrolidylidene)-3-(2,6-dimethylphenyl)urea which is dissolved in ether and converted to the hydrochloride salt. Recrystallizations from methanol yields the product, 1-(1-benzyl-2-pyrrolidylidene)-3-(2,6-dimethylphenyl)urea HCl, m.p. = 185°-195° C. (dec.)

후처리

  1. dry with materialAfter drying over K2CO3
  2. filtrationthe benzene solution is filtered through diatomaceous earth and 3.68 g
  3. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-7e2b7db0271643a595da5d3cb8399d4a
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998958

연결된 노트

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