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

HRID 451237
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HRID 451237 반응식
C([O:3][C:4](=[O:36])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([C:22]3[N:26]([CH2:27][CH2:28][O:29][CH2:30][CH3:31])[C:25]4[CH:32]=[CH:33][CH:34]=[CH:35][C:24]=4[N:23]=3)[CH2:18][CH2:17]2)=[CH:10][CH:9]=1)([CH3:7])[CH3:6])C.[OH-].[Na+].C(O)C.O>C(O)CCC.C(OC(=O)C)C.C(O)(=O)C>[CH2:30]([O:29][CH2:28][CH2:27][N:26]1[C:25]2[CH:32]=[CH:33][CH:34]=[CH:35][C:24]=2[N:23]=[C:22]1[CH:19]1[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C:11]2[CH:10]=[CH:9][C:8]([C:5]([CH3:6])([CH3:7])[C:4]([OH:36])=[O:3])=[CH:13][CH:12]=2)[CH2:17][CH2:18]1)[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 66869688Ethyl 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazole-2-yl)piperidine-1-yl)ethyl)phenyl]-2-methylpropanoate

생성물 1

HCID 185460Bilastine수율 85%

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
HCID 2631-Butanol용매
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 ethylester (2.3 g) prepared in the Example 15, sodium hydroxide (0.6 g) and ethyl alcohol (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 layers. The separated organic layer was condensed under reduced pressure. And, butanol (9 mL) was added 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 (1.84 g, yield 85%, HPLC purity 99% or more).

후처리

  1. additionwere introduced
  2. customthe mixture was reacted at 50-55□ for 3 hours
  3. customto separate layers
  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-223de2c3fdb54e6a9ffb84ecc3fab67c
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08487106B2

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