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Acetyl chloride → HCID 10517454, 화합물

HRID 1383619
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HRID 1383619 반응식
[OH:1][C@H:2]1[CH2:16][CH:15]=[C:14]2[C@:4]([CH3:17])([CH2:5][C:6]3[C:7](=[CH:13]2)[O:8][C:9](=[O:12])[C:10]=3[CH3:11])[C@H:3]1[CH3:18].[C:19](Cl)(=[O:21])[CH3:20].S([O-])(O)(=O)=O.[K+]>N1C=CC=CC=1>[C:19]([O:1][C@H:2]1[CH2:16][CH:15]=[C:14]2[C@:4]([CH3:17])([CH2:5][C:6]3[C:7](=[CH:13]2)[O:8][C:9](=[O:12])[C:10]=3[CH3:11])[C@H:3]1[CH3:18])(=[O:21])[CH3:20]
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참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 516920Potassium bisulfateHCID 10514571HCID 10514571, 화합물

생성물 1

HCID 10517454HCID 10517454, 화합물수율 80%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
25 °C

실험 절차

The compound prepared in Example B1 (in the general formula (II), R3=H, R4=CH3, and R5=H) (50 mg, 0.20 mmol) was dissolved in pyridine (5 ml), acetyl chloride (80 mg, 0.70 mmol) was added thereto, and the mixture was stirred at 25° C. for one hr. A 15% aqueous potassium hydrogensulfate solution was added to the reaction solution, followed by extraction with methylene chloride. The organic layer was washed with saturated saline and dried over magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1) to give the title compound (55 mg, 80%).

후처리

  1. extractionfollowed by extraction with methylene chloride
  2. washThe organic layer was washed with saturated saline
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-f35c0377f91243f1a1e5a65a099dcd23
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06255339B1

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