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Pyridine → HCID 131723973, 화합물

HRID 1357501
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HRID 1357501 반응식
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:10][C@:11]1([C:23]([O:25][CH3:26])=[O:24])[CH2:21][C@@H:20]([OH:22])[C@@H:14]2[O:15][C:16]([CH3:19])([CH3:18])[O:17][C@@H:13]2[CH2:12]1.N1C=CC=CC=1>ClCCl>[C:1]([O:22][C@H:20]1[C@@H:14]2[O:15][C:16]([CH3:18])([CH3:19])[O:17][C@@H:13]2[CH2:12][C@@:11]([OH:10])([C:23]([O:25][CH3:26])=[O:24])[CH2:21]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 11680350HCID 11680350, 화합물

생성물 1

HCID 131723973HCID 131723973, 화합물수율 86.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Benzoyl chloride (0.78 mL, 6.7 mmol) was added dropwise to 0° C. a solution of Example 13B (1.65 g, 6.7 mmol) and pyridine (0.82 mL, 10.1 mmol) in dichloromethane (40 mL). After stirring for 12 hours, the reaction mixture was washed with aqueous HCl (2N), saturated NaHCO3 solution, and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by flash chromatography using hexanes/ethyl acetate (3/2) to afford 2.02 g (86%) of the desired product as a white solid.

후처리

  1. washthe reaction mixture was washed with aqueous HCl (2N), saturated NaHCO3 solution, and brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe concentrate was purified by flash chromatography

출처 및 근거

ORD 기록
ord-1f61b840ec1e489db1d90cdebdf3399a
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06593314B1

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