N-Methyl-tert-butylamine → HCID 23364249, compound

HRID 1081495Notes

Reaction equation

HRID 1081495 reaction equation
[CH2:1]([O:3][C:4]1[CH:40]=[CH:39][C:7]2[N:8]([S:18]([C:21]3[CH:26]=[CH:25][C:24]([NH:27][C:28]([O:30]C4C=CC=CC=4)=O)=[CH:23][C:22]=3[O:37][CH3:38])(=[O:20])=[O:19])[C:9](=[O:17])[N:10]([CH:11]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]3)[C:6]=2[CH:5]=1)[CH3:2].[CH3:41][NH:42][C:43]([CH3:46])([CH3:45])[CH3:44]>C(Cl)Cl>[C:43]([N:42]([CH3:41])[C:28](=[O:30])[NH:27][C:24]1[CH:25]=[CH:26][C:21]([S:18]([N:8]2[C:7]3[CH:39]=[CH:40][C:4]([O:3][CH2:1][CH3:2])=[CH:5][C:6]=3[N:10]([CH:11]3[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]3)[C:9]2=[O:17])(=[O:19])=[O:20])=[C:22]([O:37][CH3:38])[CH:23]=1)([CH3:46])([CH3:45])[CH3:44]

Participants

4

Reactant 2

HCID 84552N-Methyl-tert-butylamineHCID 15231555HCID 15231555, compound

Product 1

HCID 23364249HCID 23364249, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 0.5 g of the compound obtained in EXAMPLE 16 step A), 1 ml of N-methyl-tert-butylamine and 20 ml of DCM is stirred for 2 hours at RT. The solvent is evaporated off under vacuum and the residue is chromatographed on silica using a DCM/AcOEt mixture (95/5; v/v) as the eluent to give 0.13 g of the expected product after crystallization from an iso ether/ AcOEt mixture (65/35; v/v). M.p.=208° C.

Workup

  1. customThe solvent is evaporated off under vacuum
  2. customthe residue is chromatographed on silica using a DCM/AcOEt mixture (95/5; v/v) as the eluent

Sources & evidence

ORD record
ord-a496a760af0045d798db2335368b4e18
Source dataset
uspto-grants-1996_12
Patent number
US05585394

Reaction notes

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