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HCID 58504230、化合物 → HCID 58504273、化合物

HRID 2407688
ノート
印刷プレビュー

反応式

HRID 2407688 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 58504230HCID 58504230、化合物

生成物 1

HCID 58504273HCID 58504273、化合物収率 65%

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-a72affea3a0b4381a2b307ce574c0bc4
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

反応ノート

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