4-Amino-1-Boc-piperidine → HCID 59683257, compound

HRID 2061483Notes

Reaction equation

HRID 2061483 reaction equation
[F:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[CH:5]=[C:4]([I:10])[C:3]=1[N:11]=[C:12]=[O:13].[NH2:14][CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]1>ClCCl>[F:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[CH:5]=[C:4]([I:10])[C:3]=1[NH:11][C:12]([NH:14][CH:15]1[CH2:16][CH2:17][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:19][CH2:20]1)=[O:13]

Participants

4

Reactant 2

HCID 12682914-Amino-1-Boc-piperidineHCID 59683263HCID 59683263, compound

Product 1

HCID 59683257HCID 59683257, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of the crude 2,3-difluoro-6-iodo-4-methylphenyl isocyanate from D20, 4-amino-1-N-Boc piperidine (480 mg), and dichloromethane (5 ml) was stirred at room temperature for 18 h then evaporated and directly purified by chromatography on silica gel 20 g eluting with 10-50% ethyl acetate in hexane to give the title compound, 300 mg. M−−H=494.

Workup

  1. customthen evaporated
  2. customdirectly purified by chromatography on silica gel 20 g
  3. washeluting with 10-50% ethyl acetate in hexane

Sources & evidence

ORD record
ord-8b40eba9dc2e47268446153a7809feab
Source dataset
uspto-grants-2012_10
Patent number
US08283364B2

Reaction notes

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