HCID 15550600, compound → HCID 15550601, compound

HRID 1699524Notes

Reaction equation

HRID 1699524 reaction equation
[C:1]([O:4][CH2:5][CH2:6][CH2:7][N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]2[N:21]([C:22]3[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[N:24]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH:23]=3)[C:20](=[O:36])[NH:19][C:18]=2[C:37](=O)[NH2:38])=[CH:9]1)(=[O:3])[CH3:2]>C(Cl)Cl>[C:1]([O:4][CH2:5][CH2:6][CH2:7][N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]2[N:21]([C:22]3[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[N:24]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH:23]=3)[C:20](=[O:36])[NH:19][C:18]=2[C:37]#[N:38])=[CH:9]1)(=[O:3])[CH3:2]

Participants

3

Reactant 1

HCID 15550600HCID 15550600, compound

Product 1

HCID 15550601HCID 15550601, compoundYield 82.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of 0.14 g (0.26 mmole) of the product of step b) in 7 ml of TMS-polyphosphate was heated to 50° C. for 4 hours. The mixture was diluted to 20 ml with CH2Cl2 and washed with water and brine. The organic phase was and evaporated and the residue purified by chromatography on silica (CH2Cl2:MeOH 98:2), to give 0.11 g (82%) of the sub-title compound.

Workup

  1. washwashed with water and brine
  2. customevaporated
  3. customthe residue purified by chromatography on silica (CH2Cl2:MeOH 98:2)

Sources & evidence

ORD record
ord-64ec495fdc2047f59149503a2a1bf484
Source dataset
uspto-grants-2002_02
Patent number
US06346625B1

Reaction notes

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