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Potassium Carbonate → HCID 58504138、化合物

HRID 2407787
ノート
印刷プレビュー

反応式

HRID 2407787 の反応式
[CH3:1][O:2][CH:3]([O:40][CH3:41])[CH2:4][N:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=[O:39])[CH2:19][CH2:20][CH:21]1[CH2:26][CH2:25][N:24]([CH2:27][C:28]2[S:32][C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=3)=[N:30][CH:29]=2)[CH2:23][CH2:22]1)[C:6](=O)[C:7]([O:9][CH3:10])=[O:8].C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:1][O:2][CH:3]([O:40][CH3:41])[CH2:4][N:5]1[C:12]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:18](=[O:39])[C:19]([CH2:20][CH:21]2[CH2:22][CH2:23][N:24]([CH2:27][C:28]3[S:32][C:31]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=4)=[N:30][CH:29]=3)[CH2:25][CH2:26]2)=[C:6]1[C:7]([O:9][CH3:10])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 58504269HCID 58504269、化合物

生成物 1

HCID 58504138HCID 58504138、化合物収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound prepared in Example 324 (0.390 g) was suspended in methanol (7 mL) and potassium carbonate (0.093 g) added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure to afford the crude material, which was partitioned between ethyl acetate and water. The organics were washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to afford the crude product, which was purified by flash column chromatography (eluant: 5% (9:1 methanol/concentrated ammonium hydroxide)/ethyl acetate) to furnish the title compound (0.340 g) having the following physical properties.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto afford the crude material, which
  3. customwas partitioned between ethyl acetate and water
  4. washThe organics were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto afford the crude product, which
  9. customwas purified by flash column chromatography (eluant: 5% (9:1 methanol/concentrated ammonium hydroxide)/ethyl acetate)

出典と根拠

ORDレコード
ord-49ef056f675b4fb997e8a8f4bbb545c0
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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