Dimethylformamide dimethyl acetal → HCID 53970306, compound

HRID 464520Notes

Reaction equation

HRID 464520 reaction equation
[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11](=[O:18])[CH2:10][CH2:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO[CH:21](OC)[N:22]([CH3:24])[CH3:23]>>[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11](=[O:18])[C:10](=[CH:21][N:22]([CH3:24])[CH3:23])[CH2:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

3

Reactant 2

HCID 78373Dimethylformamide dimethyl acetalHCID 12948282HCID 12948282, compound

Product 1

HCID 53970306HCID 53970306, compound

Procedure

A mixture of 5.2 g (22 mmole) of 3,4-dihydro-1-phenyl-5H-2-benzazepin-5-one and 43 ml of dimethylformamide dimethyl acetal was refluxed for 4 hr. The mixture was concentrated at reduced pressure to dryness. The residue was crystallized with ether to give a yellow solid, mp 131°-133° C. Recrystallization from ether gave yellow prisms, mp 131°-132° C.

Workup

  1. temperaturewas refluxed for 4 hr
  2. concentrationThe mixture was concentrated at reduced pressure to dryness
  3. customThe residue was crystallized with ether
  4. customto give a yellow solid, mp 131°-133° C
  5. customRecrystallization from ether
  6. customgave yellow prisms, mp 131°-132° C.

Sources & evidence

ORD record
ord-0a8690a79cac4b96a71e6a0beafff19d
Source dataset
uspto-grants-1985_10
Patent number
US04547581

Reaction notes

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