HCID 10414055, compound → HCID 23045029, compound

HRID 2108110Notes

Reaction equation

HRID 2108110 reaction equation
[CH3:1][O:2][C:3]1[C:4]([O:36][CH3:37])=[CH:5][C:6]2[O:12][CH2:11][CH2:10][C:9]([C:13]([N:15]3[CH2:20][CH2:19][N:18]([C:21](=[O:34])[C:22]4[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([O:32][CH3:33])[CH:23]=4)[CH2:17][CH2:16]3)=[O:14])=[CH:8][C:7]=2[CH:35]=1>[C].[Pd].CO>[CH3:1][O:2][C:3]1[C:4]([O:36][CH3:37])=[CH:5][C:6]2[O:12][CH2:11][CH2:10][CH:9]([C:13]([N:15]3[CH2:16][CH2:17][N:18]([C:21](=[O:34])[C:22]4[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([O:32][CH3:33])[CH:23]=4)[CH2:19][CH2:20]3)=[O:14])[CH2:8][C:7]=2[CH:35]=1

Participants

4

Reactant 1

HCID 10414055HCID 10414055, compound

Product 1

HCID 23045029HCID 23045029, compound

Reagents, catalysts & solvents 2

HCID 178418390HCID 178418390, compoundCatalystHCID 887MethanolSolvent

Procedure

A mixture of 1-(7,8-dimethoxy-2,3-dihydro-1-benzoxepin4-ylcarbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine obtained in Working Example 26 (0.5 g) and methanol (20 ml) is stirred under a hydrogen stream in the presence of 10% palladium-carbon (0.3 g) under atmospheric pressure at room temperature for 10 hours. After filtration of the catalyst, the filtrate is concentrated under reduced pressure. The residue is dissolved in ethyl acetate. The resulting solution is washed with water, dried and concentrated in vacuo. The residue is tritutated with ethyl ether and the resulting powder is filtered off to give 1-(7,8-dimethoxy2,3,4,5-tetrahydro-1-benzoxepin-4-ylcarbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine as a colorless powder (0.4 g).

Workup

  1. filtrationAfter filtration of the catalyst
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. dissolutionThe residue is dissolved in ethyl acetate
  4. washThe resulting solution is washed with water
  5. customdried
  6. concentrationconcentrated in vacuo
  7. filtrationthe resulting powder is filtered off

Sources & evidence

ORD record
ord-13c9d9012dfb49f98f3e4bf11c9aec6a
Source dataset
uspto-grants-1990_06
Patent number
US04937246

Reaction notes

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