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Hydrochloric Acid → HCID 44632534, 화합물

HRID 2362027
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HRID 2362027 반응식
[C:1](Cl)(=O)C.[Na+].[Cl-].[Cl:7][C:8]1[CH:9]=[C:10]([C:15]2[CH2:19][CH:18]([CH2:20][C:21]([OH:23])=[O:22])[O:17][N:16]=2)[CH:11]=[CH:12][C:13]=1[Cl:14].Cl>CO>[CH3:1][O:22][C:21](=[O:23])[CH2:20][CH:18]1[O:17][N:16]=[C:15]([C:10]2[CH:11]=[CH:12][C:13]([Cl:14])=[C:8]([Cl:7])[CH:9]=2)[CH2:19]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 6367Acetyl chlorideHCID 44634451HCID 44634451, 화합물

생성물 1

HCID 44632534HCID 44632534, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Acetyl chloride (5 eq) was added to MeOH (50 vol) externally cooled with a mixture saturated aqueous NaCl solution and ice. After 10 minutes the solution was warmed to room temperature. After a further 90 minutes, [3-(3,4-dichloro-phenyl)-4,5-dihydro-isoxazol-5-yl]-acetic acid (1.0 eq) in MeOH (25 vol) was added to the hydrogen chloride methanolic solution and stirred for 16 hours. The solvent was concentrated under reduced pressure and the residue was purified by flash column chromatography (eluent: [3:7] EtOAc:heptane) to afford [3-(3,4-dichloro-phenyl)-4,5-dihydro-isoxazol-5-yl]-acetic acid methyl ester.

후처리

  1. concentrationThe solvent was concentrated under reduced pressure
  2. customthe residue was purified by flash column chromatography (eluent: [3:7] EtOAc:heptane)

출처 및 근거

ORD 기록
ord-6be1496613f74244aff72747137e9b63
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691824B2

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