홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Acetone → N-(1-cyclopropylmethyl-3-pyrrolidinylmethyl)-2,3-dimethoxy-5-sulphamoyl benzamide

HRID 652781
노트
인쇄 미리보기

반응식

HRID 652781 반응식
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[CH:10][C:9]([S:14](=[O:17])(=[O:16])[NH2:15])=[CH:8][C:4]=1[C:5]([OH:7])=O.CC(C)=O.ClC(OCC(C)C)=O.[CH:30]1([CH2:33][N:34]2[CH2:38][CH2:37][CH:36]([CH2:39][NH2:40])[CH2:35]2)[CH2:32][CH2:31]1>O.C(N(CC)CC)C>[CH:30]1([CH2:33][N:34]2[CH2:38][CH2:37][CH:36]([CH2:39][NH:40][C:5](=[O:7])[C:4]3[CH:8]=[C:9]([S:14](=[O:17])(=[O:16])[NH2:15])[CH:10]=[C:11]([O:12][CH3:13])[C:3]=3[O:2][CH3:1])[CH2:35]2)[CH2:31][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 180AcetoneHCID 62365Isobutyl chloroformateHCID 30176982,3-Dimethoxy-5-sulphamoylbenzoic acidHCID 201968231-Cyclopropylmethyl-3-aminomethyl-pyrrolidine

생성물 1

HCID 54178752N-(1-cyclopropylmethyl-3-pyrrolidinylmethyl)-2,3-dimethoxy-5-sulphamoyl benzamide

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 8471Triethylamine용매

실험 절차

6.6 g of 2,3-dimethoxy-5-sulphamoyl benzoic acid, 50 ml of acetone, 10 ml of water and 3.6 ml of triethylamine (density 0.726) are placed in a 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The solution is cooled to 0°-+5° C. and 3.6 g of isobutyl chloroformate is poured in drop by drop. It is reacted for 30 minutes with the same temperature maintained, after which 4.8 g of 1-cyclopropylmethyl-3-aminomethyl-pyrrolidine is added drop by drop. The reaction medium is agitated for 1 hour at room temperature, whereupon 50 ml of water is added and the acetone evaporated under vacuum. A further 50 ml of water is added and the solution is made alkaline with 5 ml of ammonia (density=0.91). An oil is precipitated. The suspension is extracted 3 times with 50 ml of methylene chloride. The organic phase is dried over magnesium sulphate, filtered, then evaporated under vacuum. The residue is dissolved in boiling ethyl acetate. It crystallises hot. The crystals are cooled, filtered and dried in an oven at 50° C.

후처리

  1. customfitted with an agitator
  2. temperatureThe solution is cooled to 0°-+5° C.
  3. customIt is reacted for 30 minutes with the same temperature
  4. temperaturemaintained
  5. additionis added
  6. customthe acetone evaporated under vacuum
  7. additionA further 50 ml of water is added
  8. customAn oil is precipitated
  9. extractionThe suspension is extracted 3 times with 50 ml of methylene chloride
  10. dry with materialThe organic phase is dried over magnesium sulphate
  11. filtrationfiltered
  12. customevaporated under vacuum
  13. dissolutionThe residue is dissolved
  14. customIt crystallises hot
  15. temperatureThe crystals are cooled
  16. filtrationfiltered
  17. customdried in an oven at 50° C.

출처 및 근거

ORD 기록
ord-21c47a3642c341d596ed562ff6ead4cb
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04673686

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트