HCID 86748133, compound → HCID 18966533, compound

HRID 2226129Notes

Reaction equation

HRID 2226129 reaction equation
[CH3:1][N:2]([CH3:15])[CH2:3][C:4]#[C:5][CH2:6][NH:7][C:8](=[O:14])/[CH:9]=[CH:10]\[C:11]([OH:13])=O>C(Cl)Cl>[CH3:1][N:2]([CH3:15])[CH2:3][C:4]#[C:5][CH2:6][N:7]1[C:8](=[O:14])[CH:9]=[CH:10][C:11]1=[O:13]

Participants

3

Reactant 1

HCID 86748133HCID 86748133, compound

Product 1

HCID 18966533HCID 18966533, compoundYield 51.6%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A Kugelrohr oven apparatus is used to heat 1.25 g of product from Example 10 at 145°-180° C. (0.1 mm Hg) for 30 minutes. The distillate is dissolved in methylene chloride, dried over sodium sulfate, filtered and concentrated in vacuo to give 0.59 g of the product as a dark oil. The oil is redistilled at 130°-135° C. (0.05-0.075 mm Hg) to give 0.240 g of the desired product as a dark amber oil.

Workup

  1. dry with materialdried over sodium sulfate
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-0ed3e4a0b764422fb683a9fa1dc58e1c
Source dataset
uspto-grants-1994_09
Patent number
US05346910

Reaction notes

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