Ammonium formate → N-(4-tert-butylphenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

HRID 2219911노트

반응식

HRID 2219911 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[C:13]3[CH2:21][CH2:20][N:19](CC4C=CC=CC=4)[CH2:18][C:14]=3[N:15]=[CH:16][N:17]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C([O-])=O.[NH4+]>CO.O.[Pd]>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[C:13]3[CH2:21][CH2:20][NH:19][CH2:18][C:14]=3[N:15]=[CH:16][N:17]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 2

HCID 2723923Ammonium formateHCID 11383178HCID 11383178, 화합물

생성물 1

HCID 59021490N-(4-tert-butylphenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine수율 96%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 962Water용매

실험 절차

A mixture of N-(4-tert-butylphenyl)-7-benzyl-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine (0.359 g, 0.96 mmol), prepared as described in Example 2, ammonium formate (0.304 g, 4.82 mmol) and palladium (10% wt. on activated carbon, 40 mg) in MeOH (5 mL) was stirred at r.t. for one h and then at 60° C. for two h. The mixture was cooled to r.t. and filtered over celite. The filtrate was concentrated under reduced pressure to give a white solid which was dissolved in water. The mixture was extracted twice with a 3:1 mixture of chloroform:isopropanol. The combined organic extracts were dried over sodium sulfate and concentrated to dryness to give 0.26 g (96%) of the title compound which was used directly without further purification.

후처리

  1. customprepared
  2. temperatureThe mixture was cooled to r.t.
  3. filtrationfiltered over celite
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customto give a white solid which
  6. extractionThe mixture was extracted twice with a 3:1 mixture of chloroform
  7. dry with materialThe combined organic extracts were dried over sodium sulfate
  8. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-9ecade95ed244788a366e5046b992176
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07414131B2

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