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

Hydrochloric Acid → HCID 15605608, 화합물

HRID 1994173
노트
인쇄 미리보기

반응식

HRID 1994173 반응식
CC1(C)C(C)(C)OB([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[S:16][CH:17]=[CH:18][C:19]=3[NH:20][S:21]([CH:24]([CH3:26])[CH3:25])(=[O:23])=[O:22])=[CH:11][CH:10]=2)O1.C([O:30][C:31](=[O:42])[C:32]1[CH:37]=[CH:36][C:35](I)=[C:34]([O:39][CH2:40][CH3:41])[CH:33]=1)C.COCCOC.C(O)C.C([O-])([O-])=O.[Na+].[Na+].O.[OH-].[Na+].Cl.CCCCCCC.CCCCCCC.CC(C)=O>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH2:40]([O:39][C:34]1[CH:33]=[C:32]([C:31]([OH:42])=[O:30])[CH:37]=[CH:36][C:35]=1[C:9]1[CH:10]=[CH:11][C:12]([C:15]2[S:16][CH:17]=[CH:18][C:19]=2[NH:20][S:21]([CH:24]([CH3:25])[CH3:26])(=[O:22])=[O:23])=[CH:13][CH:14]=1)[CH3:41]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 10

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962Water2회HCID 80711,2-DimethoxyethaneHCID 8900HeptaneHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 21879760Acetone heptane
HCID 23090718Ethyl 3-ethoxy-4-iodobenzoate
HCID 59747992Propane-2-sulfonic acid {2-[4-(4,4,5,5-tetramethyl-[1,3,2] dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide

생성물 1

HCID 15605608HCID 15605608, 화합물수율 63.1%

시약·촉매·용매 1

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매

반응 조건

온도
60 °C

실험 절차

Mix propane-2-sulfonic acid {2-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl) -phenyl]-thiophen-3-yl}-amide (1.00 equiv; 441.02 mmoles; 196.60 g), 3-ethoxy-4-iodo -benzoic acid ethyl ester (1.00 equiv; 441.47 mmoles; 141.27 g), DME (15.15 moles; 1.57 L; 1.37 kg), PdCl2(dppf) (2.42 mmoles; 1.97 g), and ethanol (13.57 moles; 790.00 mL; 625.13 g) under a N2 atmosphere. Then add Na2CO3 2M in water (1.89 equiv; 833.06 mmoles; 416.53 mL; 504.00 g) and heat the reaction mixture to reflux until HPLC monitoring indicates reaction completion. Cool reaction mixture to RT then add water (109.13 moles; 1.97 L). Separate the organic layer, filter through diatomaceous earth, then concentrate organic layer under reduced pressure. Add ethanol (2.36 L), and remove solvent under reduced pressure. Add 3-Mercaptopropyl-functionalized Silica Gel (50.00 g), and heat to 60° C. for 30 minutes. Cool to RT then filter over diatomaceous earth. Rinse cake with ethanol, then combine ethanol washes and filtrate. Add 14% Sodium Hydroxide (4.89 moles; 1.27 L; 1.43 kg) and heat the reaction mixture at 55° C. until monitoring by HPLC indicates the end of the reaction. Cool to RT then add 7N HCl to the reaction mixture. Stir the resulting precipitate overnight. Filter the reaction mixture and wash cake with EtOH/Water (40/60-v/v) (180.78 g), EtOH (155.49 g), and n-heptane (262 g). Redissolve cake in acetone (2.18 kg) and add activated charcoal (46 g). Heat the reaction mixture at 50° C. for 30 minutes. Cool to RT, filter over diatomaceous earth (765.59 mmoles; 200.00 g), and concentrate under reduced pressure. Cool to RT, then add n-Heptane (7.73 moles; 1.13 L; 775. 00 g) and stir for 1 h. Fltere and wash cake with n-heptane/acetone 60/40 (2.58 moles; 354.79 mL) and dry under reduced pressure to yield 124 g of the title compound.

후처리

  1. temperatureto reflux until HPLC monitoring
  2. customreaction completion
  3. temperatureCool
  4. customreaction mixture to RT
  5. customSeparate the organic layer
  6. filtrationfilter through diatomaceous earth
  7. customAdd ethanol (2.36 L), and remove solvent under reduced pressure
  8. temperatureCool to RT
  9. filtrationthen filter over diatomaceous earth
  10. washRinse cake with ethanol
  11. temperatureheat the reaction mixture at 55° C. until monitoring by HPLC
  12. customthe end of the reaction
  13. temperatureCool to RT
  14. filtrationFilter the reaction mixture
  15. washwash cake with EtOH/Water (40/60-v/v) (180.78 g), EtOH (155.49 g), and n-heptane (262 g)
  16. dissolutionRedissolve cake in acetone (2.18 kg)
  17. additionadd activated charcoal (46 g)
  18. temperatureHeat the reaction mixture at 50° C. for 30 minutes
  19. temperatureCool to RT
  20. filtrationfilter over diatomaceous earth (765.59 mmoles; 200.00 g)
  21. concentrationconcentrate under reduced pressure
  22. temperatureCool to RT
  23. customdry under reduced pressure

출처 및 근거

ORD 기록
ord-9e6bb47e97ed42278b0dcc1fa3022cc0
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652064B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트