Ammonium formate → HCID 11486612, 화합물

HRID 411291노트

반응식

HRID 411291 반응식
C([N:8]1[CH2:13][CH2:12][C:11]([CH2:20][N:21]([CH3:37])[C:22]2[N:31]=[C:30]([NH2:32])[C:29]3[C:24](=[CH:25][C:26]([O:35][CH3:36])=[C:27]([O:33][CH3:34])[CH:28]=3)[N:23]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.O.[Pd]>[CH3:34][O:33][C:27]1[CH:28]=[C:29]2[C:24](=[CH:25][C:26]=1[O:35][CH3:36])[N:23]=[C:22]([N:21]([CH2:20][C:11]1([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)[CH3:37])[N:31]=[C:30]2[NH2:32]

참가 물질

6

반응물 2

HCID 2723923Ammonium formateHCID 11294944HCID 11294944, 화합물

생성물 1

HCID 11486612HCID 11486612, 화합물수율 75.1%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of N2-(1-Benzyl-4-phenyl-piperidin-4-ylmethyl)-6,7-dimethoxy-N2-methyl-quinazoline-2,4-diamine 10, (1.3 g) and ammonium formate (2.2 g) in 24 ml methanol and 6 ml water was added 10% Pd-C (250 mg). After stirring under reflux for two hours, the reaction mixture was cooled and filtered through celite®. The filtrate was concentrated to a small volume, made basic with potassium carbonate, and extracted with dichloromethane. The extract was dried over potassium carbonate, filtered, and evaporated. The residue was chromatographed on silica gel to provide 800 mg of 6,7-dimethoxy-N2-(4-phenyl-piperidin-4-ylmethyl)-N2-methyl-quinazoline-2,4-diamine 11 as a white powder, MS: 407 (M+).

후처리

  1. temperatureunder reflux for two hours
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered through celite®
  4. concentrationThe filtrate was concentrated to a small volume
  5. extractionextracted with dichloromethane
  6. dry with materialThe extract was dried over potassium carbonate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-cc7fd09e00924a6aba162119c87d9c9f
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559153B2

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