Ammonia → HCID 13151854, compound

HRID 1075024Notes

Reaction equation

HRID 1075024 reaction equation
[O:1]=[C:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[S:5][C:4]2[CH:13]=[C:14]([C:17](OC)=O)[CH:15]=[CH:16][C:3]1=2.[NH3:21]>CO>[C:17]([C:14]1[CH:15]=[CH:16][C:3]2[C:2](=[O:1])[CH2:8][C:7]3[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=3[S:5][C:4]=2[CH:13]=1)#[N:21]

Participants

4

Reactant 2

HCID 222AmmoniaHCID 20270213HCID 20270213, compound

Product 1

HCID 13151854HCID 13151854, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Stir 5 gm. of methyl 10,11-dihydro-11-oxodibenzo[b,f]thiepin-3-carboxylate in 500 ml. of methanol saturated with ammonia gas for 24 hours at room temperature. Evaporate the reaction mixture to dryness. Reflux the residue in 200 ml. of methylene chloride containing 10 gm. of phosphorous oxychloride for eight hours. Cool the reaction mixture to room temperature and shake several times with water. Separate the organic layer, dry over magnesium sulfate and evaporate to dryness to obtain the title product.

Workup

  1. customEvaporate the reaction mixture to dryness
  2. temperatureReflux the residue in 200 ml
  3. customSeparate the organic layer
  4. dry with materialdry over magnesium sulfate
  5. customevaporate to dryness

Sources & evidence

ORD record
ord-59e98e0b9c8a4e64b872fa4b2bdaa804
Source dataset
uspto-grants-1983_07
Patent number
US04394515

Reaction notes

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