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HCID 58906458, 화합물 → Tert-butyl 4-methoxy-4-((methylamino)methyl)piperidine-1-carboxylate

HRID 1294582
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HRID 1294582 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([CH2:16][N:17](CC2C=CC=CC=2)[CH3:18])([O:14][CH3:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(OCC)(=O)C.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][C:11]([O:14][CH3:15])([CH2:16][NH:17][CH3:18])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 1

HCID 58906458HCID 58906458, 화합물

생성물 1

HCID 58906435Tert-butyl 4-methoxy-4-((methylamino)methyl)piperidine-1-carboxylate수율 86%

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 8857Ethyl Acetate용매

실험 절차

Amine (36) (55 g, 158 mmol) was dissolved in ethyl acetate (500 ml). Pd—C (10%, wet, 5 g) was added and the mixture was stirred for 23 h under hydrogen atmosphere (1 bar). TLC analysis revealed incomplete conversion. Extra Pd—C (2.5 g) was added and the mixture was stirred under H2 (1 bar) for 110 h. NMR analysis revealed complete conversion. The mixture was filtrated over Celite, the Celite crop was washed with ethyl acetate and the filtrate was evaporated to dryness. The residue was purified by distillation (bulb to bulb, 0.04 mbar, 130° C.) giving 35 g of compound (37) (86%) as colorless oil.

후처리

  1. stirringthe mixture was stirred under H2 (1 bar) for 110 h
  2. filtrationThe mixture was filtrated over Celite
  3. washthe Celite crop was washed with ethyl acetate
  4. customthe filtrate was evaporated to dryness
  5. distillationThe residue was purified by distillation (bulb to bulb, 0.04 mbar, 130° C.)

출처 및 근거

ORD 기록
ord-d0b2ac0b9ca14da9a693a28c02d6dc1c
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07241770B2

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