Formaldehyde → HCID 21419181, compound

HRID 441505Notes

Reaction equation

HRID 441505 reaction equation
[CH3:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5][O:4][NH:3]1.[CH2:13]=O>C(O)=O>[CH3:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5][O:4][N:3]1[CH3:13]

Participants

4

Reactant 2

HCID 712FormaldehydeHCID 21419172HCID 21419172, compound

Product 1

HCID 21419181HCID 21419181, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent

Procedure

To 1.1 ml. of 99 percent formic acid, 1 g. (0.0061 mole) of 1-methyl-1,2,4,5-tetrahydro-3,2-benzoxazepine and 0.45 ml. of 38 percent formaldehyde were added. After heating the reaction mixture at 60°-70° C. for about 6 hours, the excess of formic acid was distilled off. The residue was alkalinized with sodium carbonate and then extracted several times with diethyl ether. After washing with water and drying, the organic solution was evaporated. The residue was distilled at 60° C./0.1 mm Hg, giving 0.6 g. of 1,2-diemthyl-1,2,4,5-tetrahydro-3,2-benzoxazepine.

Workup

  1. temperatureAfter heating the reaction mixture at 60°-70° C. for about 6 hours
  2. distillationthe excess of formic acid was distilled off
  3. extractionextracted several times with diethyl ether
  4. washAfter washing with water
  5. customdrying
  6. customthe organic solution was evaporated
  7. distillationThe residue was distilled at 60° C./0.1 mm Hg
  8. customgiving 0.6 g

Sources & evidence

ORD record
ord-41bdea12465947afa3c7793695cc8da7
Source dataset
uspto-grants-1977_08
Patent number
US04041048

Reaction notes

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