Ammonium formate → HCID 67240315, 화합물

HRID 1520766노트

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HRID 1520766 반응식
C1(C(=[N:14][C:15]2[CH:20]=[CH:19][C:18]([C@H:21]3[O:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]3)=[CH:17][CH:16]=2)C2C=CC=CC=2)C=CC=CC=1.C([O-])=O.[NH4+]>CO.[Pd]>[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([C@H:21]2[O:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]2)=[CH:17][CH:16]=1

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 86654631HCID 86654631, 화합물

생성물 1

HCID 67240315HCID 67240315, 화합물수율 80.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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온도
60 °C

실험 절차

A suspension of (R)-tert-butyl 2-(4-(diphenylmethyleneamino)phenyl)morpholine-4-carboxylate (6 g, 13.6 mmol), ammonium formate (12.8 g, 203 mmol) and Pd/C5% (721 mg, 0.339 mmol) in methanol (103 ml) was stirred at 60° C. for 2 h. The reaction mixture was filtered and concentrated. The residue was dissolved in ethyl acetate and water. The organic phase was extracted twice with 0.5M HCl. The combined aqueous phases were basified with 2M-NaOH and extracted twice with DCM. The organic phases were dried over magnesium sulfate, filtered and dried in vacuo, to yield 3.04 g off-white solid. MS (ISP): 279.1 ([M+H]+).

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. extractionThe organic phase was extracted twice with 0.5M HCl
  5. extractionextracted twice with DCM
  6. dry with materialThe organic phases were dried over magnesium sulfate
  7. filtrationfiltered
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-35d316cadbc74d4499e236aa56a5c87b
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073911B2

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