tert-butyl N'-(quinolin-2-yl)methylene-hydrazinecarboxylate → HCID 69200678, 화합물

HRID 2113479

반응식

HRID 2113479 반응식
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11]=[N:12][NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15]>CO.[Pd]>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][NH:12][NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15]

참가 물질

4

반응물 1

HCID 69201455tert-butyl N'-(quinolin-2-yl)methylene-hydrazinecarboxylate

생성물 1

HCID 69200678HCID 69200678, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

0.5 g 10% Pd/C are added to a solution of 15.00 g tert-butyl N′-(quinolin-2-yl)methylene-hydrazinecarboxylate in 200 ml of methanol. The resulting mixture is then shaken for 6 h at ambient temperature under 1 atm H2 pressure. Then the precipitate and the catalyst are separated from the solvent, the precipitate is dissolved in tetrahydrofuran, filtered again and in this way the catalyst is separated off. The THF solution is evaporated down and the residue is triturated with tert-butylmethylether, separated off and dried at 50° C. The tert-butylmethylether phase is evaporated down again and the residue is triturated this time with diethyl ether, separated off and dried at 50° C. The two solid fractions from the purification with tert-butylmethylether and diethyl ether are combined.

후처리

  1. customThen the precipitate and the catalyst are separated from the solvent
  2. dissolutionthe precipitate is dissolved in tetrahydrofuran
  3. filtrationfiltered again and in this way the catalyst
  4. customis separated off
  5. customThe THF solution is evaporated down
  6. customthe residue is triturated with tert-butylmethylether
  7. customseparated off
  8. customdried at 50° C
  9. customThe tert-butylmethylether phase is evaporated down again
  10. customthe residue is triturated this time with diethyl ether
  11. customseparated off
  12. customdried at 50° C
  13. customThe two solid fractions from the purification with tert-butylmethylether and diethyl ether

출처 및 근거

ORD 기록
ord-c58c2792fe6d4d1abb12e2f0d8cd9013
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432262B2

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