Dichloromethane → HCID 23462907, compound

HRID 2286412Notes

Reaction equation

HRID 2286412 reaction equation
[CH3:1][O:2][C:3]1[C:13]([O:14][CH3:15])=[CH:12][C:6]2[CH2:7][CH2:8][NH:9][CH2:10][CH2:11][C:5]=2[C:4]=1[S:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(Cl)Cl.[CH:26]1([C:29](Cl)=[O:30])[CH2:28][CH2:27]1>C(N(CC)CC)C>[CH:26]1([C:29]([N:9]2[CH2:8][CH2:7][C:6]3[CH:12]=[C:13]([O:14][CH3:15])[C:3]([O:2][CH3:1])=[C:4]([S:16][C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)[C:5]=3[CH2:11][CH2:10]2)=[O:30])[CH2:28][CH2:27]1

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 77637Cyclopropanecarbonyl chlorideHCID 23462864HCID 23462864, compound

Product 1

HCID 23462907HCID 23462907, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

To a solution of 1.58 g. (0.005 mole) of 7,8-dimethoxy-6-phenylthio-2,3,4,5-tetrahydro-1H-3-benzazepine in 25 ml. of methylene chloride and 1.0 g. of triethylamine is added dropwise 1.05 g. (0.010 mole) of cyclopropanecarboxylic acid chloride at 5° C. and the mixture is stirred at room temperature for 3 hours. The reaction mixture is filtered and the filtrate is washed with water, 5% potassium carbonate solution and then with water, dried and subsequently concentrated to give 3-cyclopropanecarbonyl-7,8-dimethoxy-6-phenylthio-2,3,4,5-tetrahydro-1H-3-benzazepine.

Workup

  1. filtrationThe reaction mixture is filtered
  2. washthe filtrate is washed with water, 5% potassium carbonate solution
  3. dry with materialwith water, dried
  4. concentrationsubsequently concentrated

Sources & evidence

ORD record
ord-bebb8fa40edc4e46bea875ce3b635989
Source dataset
uspto-grants-1981_05
Patent number
US04265890

Reaction notes

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