Methylamine → HCID 10316869, compound

HRID 2382225Notes

Reaction equation

HRID 2382225 reaction equation
Cl[CH2:2][CH2:3][C@@H:4]([O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[I:18])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH3:19][NH2:20]>C(O)C>[CH3:19][NH:20][CH2:2][CH2:3][C@@H:4]([O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[I:18])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Participants

4

Procedure

Compound 1-A (2.68 g, 7.2 mmole) was dissolved in an aqueous solution of ethanol (80 ml) and methylamine (160 ml), and heated to reflux for 30 h. After cooling, the solution was extracted with chloroform (100 ml, twice), and an organic layer was decanted. The organic layer was dried over anhydrous sodium sulfate, and dried by evaporation under vacuum, to obtain the product as oil (2.75 g, 97.4%).

Workup

  1. temperatureheated
  2. temperatureto reflux for 30 h
  3. temperatureAfter cooling
  4. extractionthe solution was extracted with chloroform (100 ml
  5. customtwice), and an organic layer was decanted
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customdried by evaporation under vacuum

Sources & evidence

ORD record
ord-9ea7b392a9ea418592cc53c4356f519e
Source dataset
uspto-grants-2012_09
Patent number
US08258331B2

Reaction notes

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