Water → Bmy 25368

HRID 1651422ノート

反応式

HRID 1651422 の反応式
C([O:5][C:6]1[C:9](=[O:10])[C:8](=O)[C:7]=1[NH:12][CH2:13][CH2:14][CH2:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)[CH:18]=1)CCC.[OH-].[NH4+:31].O>CO>[NH2:31][C:8]1[C:9](=[O:10])[C:6](=[O:5])[C:7]=1[NH:12][CH2:13][CH2:14][CH2:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)[CH:18]=1

参加物

5

反応物 3

HCID 962WaterHCID 14923Ammonium HydroxideHCID 150787681-Butoxy-2-[3-(3-piperidinomethylphenoxy)propylamino]-1-cyclobutene-3,4-dione

生成物 1

HCID 135156Bmy 25368収率 77%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-butoxy-2-[3-(3-piperidinomethylphenoxy)propylamino]-1-cyclobutene-3,4-dione [prepared in Example 2] (4.06 g, 0.01014 mole) in methanol (40 mL) was added 14M aqueous ammonium hydroxide (1.5 mL, 0.021 mole). The mixture was stirred at ambient temperature for 41 hours. Water (40 mL) was added and stirring was continued for 10 minutes. The precipitate was collected by filtration, washed with methanol:water (1:1) (20 mL), and dried in vacuo to give 2.68 g (77.0% yield) of the title compound. A sample purified by chromatography showed spectral data identical to that of an authentic sample.

後処理

  1. stirringstirring
  2. waitwas continued for 10 minutes
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with methanol:water (1:1) (20 mL)
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-17bb904f0c4b490bb70e3fc84b810ad3
出典データセット
uspto-grants-1990_05
特許番号
US04927970

反応ノート

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