Monomethylamine methanol → HCID 66941283, compound

HRID 348638Notes

Reaction equation

HRID 348638 reaction equation
[C:1]([O:5][C:6](=[O:42])[N:7]([CH2:27][CH2:28][CH2:29][CH2:30][NH:31][C:32]([O:34][CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:33])[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][N:16]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:11][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].CN.CO>>[C:1]([O:5][C:6](=[O:42])[N:7]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][NH2:16])=[CH:11][CH:10]=1)[CH2:27][CH2:28][CH2:29][CH2:30][NH:31][C:32]([O:34][CH2:35][C:36]1[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=1)=[O:33])([CH3:4])([CH3:2])[CH3:3]

Participants

3

Reactant 2

HCID 57454252Monomethylamine methanolHCID 66941505HCID 66941505, compound

Product 1

HCID 66941283HCID 66941283, compoundYield 74%

Procedure

The compound (173 mg) obtained in Example 42-2 was added with a 40% methylamine/methanol solution (3.0 ml), followed by stirring at room temperature for 14 hours. After completion of the reaction, the solvent was distilled off and the residue was then added with a 1 mol/l sodium hydroxide aqueous solution, followed by extraction with chloroform. The extract was dried with anhydrous sodium sulfate. Subsequently, the solvent was distilled off, thereby obtaining the subject compound (98.9 mg) as a colorless viscous liquid.

Workup

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionthe residue was then added with a 1 mol/l sodium hydroxide aqueous solution
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe extract was dried with anhydrous sodium sulfate
  6. distillationSubsequently, the solvent was distilled off

Sources & evidence

ORD record
ord-16544765c91b485fbe1976dd69c95130
Source dataset
uspto-grants-2007_02
Patent number
US07176227B2

Reaction notes

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