반응 #336536

ord-2860f9933dfa489fa051731091be82e3

반응 방정식

CC1CC2C=CC=C3OCOC312.Cc1ccc(S(=O)(=O)O)cc1
compound
CC1CC2C=CC=C3OCOC312.Cc1ccc(S(=O)(=O)O)cc1
1-methyl-3,4-methylenedioxybenzocyclobutene tosylate
CCOC(=O)N(C)C1CCNCC1
compound
CCOC(=O)N(C)C1CCNCC1
Ethyl N-piperid-4-yl-N-methylcarbamate
OCCN(CCO)CCO
triethanolamine
CCOC(=O)N(C)C1CCN(CC2=Cc3c2ccc2c3OCO2)CC1
ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture is concentrated
  2. 2
    세척washed with water
  3. 3
    추출extracted with 1 N hydrochloric acid
  4. 4
    추출extracted with methylene chloride
  5. 5
    기타The extract is dried

실험 절차

4 g of the compound obtained in Stage H, 2.24 g of the compound obtained in Stage B of Example 6 and 1.7 ml of triethanolamine are refluxed in 40 ml of toluene for 24 hours. The reaction mixture is concentrated, taken up in ethyl acetate, washed with water and then extracted with 1 N hydrochloric acid, and the extract is rendered basic with concentrated sodium hydroxide solution and extracted with methylene chloride. The extract is dried to yield ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate. 23.5 ml of a 2% solution of fumaric acid in ethanol are added to yield the desired salt.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05214055uspto-grants-1993_05