3-[[2-[2-(3,4-Dimethoxyphenyl)ethylamino]-2-oxoethyl]amino]benzamide → 2-(3-carbamoylphenylamino)-N-(3,4-dimethoxyphenethyl)acetamide trihydrate

HRID 848735Notes

Reaction equation

HRID 848735 reaction equation
[C:1]([C:4]1[CH:5]=[C:6]([NH:10][CH2:11][C:12]([NH:14][CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[CH:18]=2)=[O:13])[CH:7]=[CH:8][CH:9]=1)(=[O:3])[NH2:2]>O>[OH2:3].[OH2:3].[OH2:3].[C:1]([C:4]1[CH:5]=[C:6]([NH:10][CH2:11][C:12]([NH:14][CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[CH:18]=2)=[O:13])[CH:7]=[CH:8][CH:9]=1)(=[O:3])[NH2:2]

Participants

3

Reactant 1

HCID 1566513-[[2-[2-(3,4-Dimethoxyphenyl)ethylamino]-2-oxoethyl]amino]benzamide

Product 1

HCID 221497912-(3-carbamoylphenylamino)-N-(3,4-dimethoxyphenethyl)acetamide trihydrateYield 225.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 0.2 g of pulverized 2-(3-carbamoylphenylamino)-N-(3,4-dimethoxyphenethyl)acetamide was added 100 ml of water and the mixture was stirred at 60° to 65° C. for 30 minutes to dissolve the powder completely. The solution was then concentrated under reduced pressure at 60° C. until about 40 ml of residual liquid was left, and allowed to stand at room temperature overnight. The colorless needles precipitated were collected by filtration, washed with water and then air-dried by allowing to stand at room temperature to obtain 0.13 g of 2-(3-carbamoylphenylamino)-N-(3,4-dimethoxyphenethyl)acetamide trihydrate having a melting point of 54°-57° C.

Workup

  1. dissolutionto dissolve the powder completely
  2. concentrationThe solution was then concentrated under reduced pressure at 60° C. until about 40 ml of residual liquid
  3. waitwas left
  4. waitto stand at room temperature overnight
  5. customThe colorless needles precipitated
  6. filtrationwere collected by filtration
  7. washwashed with water
  8. customair-dried
  9. customto stand at room temperature

Sources & evidence

ORD record
ord-f584edcc0fe4495a936c2f46d3771082
Source dataset
uspto-grants-1981_10
Patent number
US04297357

Reaction notes

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