HCID 58504230, 화합물 → HCID 58504273, 화합물

HRID 2407688노트

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HRID 2407688 반응식
[Cl:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[N:9][O:10][C:6]=2[C:5](NN)=[N:4][N:3]=1>C1C=CC=CC=1.C(O)C.[OH-].[Na+]>[Cl:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[N:9][O:10][C:6]=2[CH:5]=[N:4][N:3]=1

참가 물질

5

반응물 1

HCID 58504230HCID 58504230, 화합물

생성물 1

HCID 58504273HCID 58504273, 화합물수율 65%

시약·촉매·용매 3

HCID 241Benzene용매HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

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온도
0 °C

실험 절차

The compound prepared in Example 81 (4.40 g) was dissolved in benzene (500 mL)-ethanol (50 mL) and 1 mol/L aqueous sodium hydroxide (67.0 mL) was added. This mixture was cooled to 0° C. Oxygen was bubbled through the vigorously stirred mixture for 30 minutes. The mixture was separated and the aqueous portion was extracted with dichloromethane. The combined organics were washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1) to obtain the title compound (2.53 g) having the following physical data.

후처리

  1. additionwas added
  2. customOxygen was bubbled through the vigorously stirred mixture for 30 minutes
  3. customThe mixture was separated
  4. extractionthe aqueous portion was extracted with dichloromethane
  5. washThe combined organics were washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-a72affea3a0b4381a2b307ce574c0bc4
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809538B2

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