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Sodium Bicarbonate → HCID 58947962, 화합물

HRID 1160143
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HRID 1160143 반응식
[NH2:1][C:2]1([CH2:8][S:9]([N:12]([CH3:14])[CH3:13])(=[O:11])=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[C:15](=O)(O)[O-:16].[Na+]>ClCCl>[N:1]([C:2]1([CH2:8][S:9]([N:12]([CH3:14])[CH3:13])(=[O:11])=[O:10])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1)=[C:15]=[O:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 58947953HCID 58947953, 화합물

생성물 1

HCID 58947962HCID 58947962, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A solution of amine hydrochloride 1200-D (520 mg) in 40 mL of dichloromethane was treated with 20 mL of aqueous saturated sodium bicarbonate solution and stirred vigorously for 10 min at 0° C. Stirring was stopped and layers were allowed to separate. Phosgene (10 mL of 20% solution in toluene) was added to the organic layer (lower layer) in one portion. The mixture was vigorously stirred immediately after addition for 10 min at 0° C. and further stirred at room temp for 3 h. The mixture was diluted with 100 mL of dichloromethane and layers were separated. The organic layer was washed with 50 mL of cold aqueous saturated sodium bicarbonate solution and dried over magnesium sulfate. The organic layer was filtered and diluted with 15 mL of toluene. The resulting solution was concentrated under reduced pressure and the product 1200-E was maintained as a 0.2M solution.

후처리

  1. stirringStirring
  2. customto separate
  3. additionPhosgene (10 mL of 20% solution in toluene) was added to the organic layer (lower layer) in one portion
  4. stirringThe mixture was vigorously stirred immediately
  5. additionafter addition for 10 min at 0° C.
  6. stirringfurther stirred at room temp for 3 h
  7. additionThe mixture was diluted with 100 mL of dichloromethane and layers
  8. customwere separated
  9. washThe organic layer was washed with 50 mL of cold aqueous saturated sodium bicarbonate solution
  10. dry with materialdried over magnesium sulfate
  11. filtrationThe organic layer was filtered
  12. additiondiluted with 15 mL of toluene
  13. concentrationThe resulting solution was concentrated under reduced pressure
  14. temperaturethe product 1200-E was maintained as a 0.2M solution

출처 및 근거

ORD 기록
ord-2c628f6bd0454db99010382641ffa855
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816326B2

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