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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanol → Bilastine

HRID 472805
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인쇄 미리보기

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HRID 472805 반응식
C[O:2][C:3](=[O:35])[C:4]([C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][CH:18]([C:21]3[N:25]([CH2:26][CH2:27][O:28][CH2:29][CH3:30])[C:24]4[CH:31]=[CH:32][CH:33]=[CH:34][C:23]=4[N:22]=3)[CH2:17][CH2:16]2)=[CH:9][CH:8]=1)([CH3:6])[CH3:5].[OH-].[Na+].C(O)C.O>C(O)CCC.C(OC(=O)C)C.C(O)(=O)C>[CH2:29]([O:28][CH2:27][CH2:26][N:25]1[C:24]2[CH:31]=[CH:32][CH:33]=[CH:34][C:23]=2[N:22]=[C:21]1[CH:18]1[CH2:19][CH2:20][N:15]([CH2:14][CH2:13][C:10]2[CH:9]=[CH:8][C:7]([C:4]([CH3:5])([CH3:6])[C:3]([OH:35])=[O:2])=[CH:12][CH:11]=2)[CH2:16][CH2:17]1)[CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 45257628Bilastine Ester

생성물 1

HCID 185460Bilastine수율 90%

시약·촉매·용매 3

HCID 176Acetic Acid용매
HCID 263
1-Butanol
용매
HCID 8857Ethyl Acetate용매

실험 절차

In a reaction vessel, 2-[4-(2-{4-[1-(2-ethoxy-ethyl)-1H-benzoimidazol-2-yl]-piperidin-1-yl}-ethyl)-phenyl]-2-methyl-propionic acid methylester (2.3 g) prepared in the Example 14, sodium hydroxide (0.6 g) and ethylalcohol (13 mL) were introduced, and the mixture was reacted at 50-55□ for 3 hours. Distilled water (20 mL) was added thereto, and acetic acid was added to control the pH to 7. Ethylacetate (50 mL) was added thereto, and the mixture was stirred to separate a layer. The separated organic layer was condensed under reduced pressure. And, butanol (9 mL) was added thereto, and dissolved by heating. And then, it was cooled to precipitate crystals, and the crystals were filtered under reduced pressure to obtain 2-[4-(2-{4-[1-(2-ethoxy-ethyl)-1H-benzoimidazol-2-yl]-piperidin-1-yl}-ethyl)-phenyl]-2-methyl-propionic acid (2.0 g, yield 90%, HPLC purity 99% or more).

후처리

  1. additionwere introduced
  2. customthe mixture was reacted at 50-55□ for 3 hours
  3. customto separate a layer
  4. customcondensed under reduced pressure
  5. dissolutiondissolved
  6. temperatureby heating
  7. temperatureAnd then, it was cooled
  8. customto precipitate crystals
  9. filtrationthe crystals were filtered under reduced pressure

출처 및 근거

ORD 기록
ord-16b4eb0016594c93ae8dd1956981bc36
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633223B2

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