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Hydrochloric Acid → HCID 15605608、化合物

HRID 1994173
ノート
印刷プレビュー

反応式

HRID 1994173 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

12

反応物 10

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962Water2 回HCID 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

生成物 1

HCID 15605608HCID 15605608、化合物収率 63.1%

試薬・触媒・溶媒 1

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

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e6bb47e97ed42278b0dcc1fa3022cc0
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07652064B2

反応ノート

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