Potassium Carbonate → HCID 86630319, 화합물

HRID 19509노트

반응식

HRID 19509 반응식
[CH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][N:2]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:17][S:18]([O:21][CH2:22][CH2:23][S:24][S:25][CH2:26][CH2:27]OS(C)(=O)=O)(=[O:20])=[O:19]>C(#N)C>[CH3:17][S:18]([O-:21])(=[O:20])=[O:19].[CH3:17][S:18]([O-:21])(=[O:20])=[O:19].[S:25]([CH2:26][CH2:27][N+:2]1[CH:3]=[CH:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:1]=1)[S:24][CH2:23][CH2:22][N+:2]1[CH:3]=[CH:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:1]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1190105,6,7,8-TetrahydroisoquinolineHCID 231172092-Methanesulfonyloxyethyl disulfide

생성물 1

HCID 86630319HCID 86630319, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

반응 조건

온도
80 °C

실험 절차

3.2 g of 5,6,7,8-tetrahydroisoquinoline and 0.7 g of potassium carbonate were mixed in 3 ml of acetonitrile and brought to 80° C. A solution of 3.4 g of disulfanediyldiethane-2,1-diyl dimethane sulfonate in 3 ml of acetonitrile was added in 10 min. Stirring was maintained for 8 h at 80° C. and then the reaction medium was brought back to ambient temperature, filtered, and concentrated under vacuum. 6 ml of dichloromethane were added and the solution was poured dropwise into 500 ml of ethyl ether. The oil that had been separated by settling out was reprocessed twice by diluting in 6 ml of methanol and adding to 500 ml of ethyl ether, and a final time by diluting in 6 ml of dichloromethane and adding to 500 ml of ethyl ether. After drying under vacuum, 5.2 g of brown solid were recovered. The analyses were in compliance with the expected structure.

후처리

  1. custombrought to 80° C
  2. customwas brought back to ambient temperature
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. addition6 ml of dichloromethane were added
  6. additionthe solution was poured dropwise into 500 ml of ethyl ether
  7. customThe oil that had been separated
  8. additionby diluting in 6 ml of methanol
  9. additionadding to 500 ml of ethyl ether
  10. additiona final time by diluting in 6 ml of dichloromethane
  11. additionadding to 500 ml of ethyl ether
  12. dry with materialAfter drying under vacuum, 5.2 g of brown solid
  13. customwere recovered

출처 및 근거

ORD 기록
ord-cd1ca81fc66c4efbb1f88f5beb425df2
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07744657B2

반응 노트

불러오는 중…