Water → Ethyl 5,6-dihydro-5-methyl-11-oxodibenz[b,e]azepine-2-acetate

HRID 904188Notes

Reaction equation

HRID 904188 reaction equation
[CH3:1][N:2]([CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]#N)[C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1.[OH2:24]>>[CH3:1][N:2]1[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22](=[O:24])[C:4]2[CH:5]=[C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:7]=[CH:8][C:3]1=2

Participants

3

Reactant 2

HCID 962WaterHCID 23333579HCID 23333579, compound

Product 1

HCID 23333640Ethyl 5,6-dihydro-5-methyl-11-oxodibenz[b,e]azepine-2-acetate

Procedure

A mixture of N-methyl-N-(2-cyanobenzyl)-4-ethoxycarbonylmethylaniline (6 g) and polyphosphoric acid (60 g) was stirred for 2 hours with heating at 130°-140° C. After the reaction, the reaction mixture was poured into iced water (500 ml) to precipitate crystals. The crystals were collected, washed in water, and then vacuum-dried over diphosphorus pentoxide to obtain the desired compound (2.5 g) as yellow prismatic crystals.

Workup

  1. temperaturewith heating at 130°-140° C
  2. customAfter the reaction
  3. customto precipitate crystals
  4. customThe crystals were collected
  5. washwashed in water
  6. dry with materialvacuum-dried over diphosphorus pentoxide

Sources & evidence

ORD record
ord-805cb1eb3880451b9d72bcd3e1df8a71
Source dataset
uspto-grants-1980_10
Patent number
US04230703

Reaction notes

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