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Hydrochloric Acid → HCID 58975136, 화합물

HRID 737021
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반응식

HRID 737021 반응식
C[O:2][C:3](=[O:27])[C:4]1[CH:9]=[CH:8][C:7]([S:10]([N:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15]([CH:22]3[CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:14]2)(=[O:12])=[O:11])=[CH:6][CH:5]=1.[OH-].[Na+].Cl>C1COCC1>[CH:22]1([C:15]2[C:16]3[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=3)[N:13]([S:10]([C:7]3[CH:8]=[CH:9][C:4]([C:3]([OH:27])=[O:2])=[CH:5][CH:6]=3)(=[O:12])=[O:11])[CH:14]=2)[CH2:23][CH2:24][CH2:25][CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58975006HCID 58975006, 화합물

생성물 1

HCID 58975136HCID 58975136, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 12 L RBF, charge 4-(3-cyclopentyl-indole-1-sulfonyl)-benzoic acid methyl ester (465 g 1.213 mol) and THF (4.7 L). Add 5N NaOH (485 ml) dropwise at ambient temperature. Stir the solution at room temperature overnight. Bring the pH of the reaction to 1 with c.HCl. Separate the layers and extract the aqueous layer with ethyl acetate (4 L). Dry the combined organic layers over sodium sulfate, filter and rinse with ethyl acetate. Concentrate the organics under vacuum to give an off-white solid (401 g, yield=89.5%) of the title compound.

후처리

  1. customBring the pH of the reaction to 1 with c
  2. customSeparate the layers
  3. extractionextract the aqueous layer with ethyl acetate (4 L)
  4. dry with materialDry the combined organic layers over sodium sulfate
  5. filtrationfilter
  6. washrinse with ethyl acetate
  7. concentrationConcentrate the organics under vacuum

출처 및 근거

ORD 기록
ord-64b66e5cfebe480083b54db924e27f73
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07595339B2

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