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Hydroxyamine hydrochloride → HCID 178450882、化合物

HRID 2383309
ノート
印刷プレビュー

反応式

HRID 2383309 の反応式
[CH2:1]([O:5][C:6](=[O:28])[CH2:7][CH:8]1[C:17]2[C:12](=[C:13]([CH3:20])[C:14]([C:18]#[N:19])=[CH:15][CH:16]=2)[CH2:11][CH2:10][N:9]1[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:2][CH2:3][CH3:4].Cl.[NH2:30][OH:31].C(=O)(O)[O-].[Na+]>C(O)C>[CH2:1]([O:5][C:6](=[O:28])[CH2:7][CH:8]1[C:17]2[C:12](=[C:13]([CH3:20])[C:14]([C:18]([NH:30][OH:31])=[NH:19])=[CH:15][CH:16]=2)[CH2:11][CH2:10][N:9]1[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:2][CH2:3][CH3:4]
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 3

HCID 443297Hydroxyamine hydrochloride2 回HCID 516892Sodium BicarbonateHCID 595910861,1-Dimethylethyl 1-[2-(butyloxy)-2-oxoethyl]-6-cyano-5-methyl-3,4-dihydro-2(1H)-isoquinolinecarboxylate

生成物 1

HCID 178450882HCID 178450882、化合物収率 85.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

A flask was charged with 1,1-dimethylethyl 1-[2-(butyloxy)-2-oxoethyl]-6-cyano-5-methyl-3,4-dihydro-2(1H)-isoquinolinecarboxylate (Preparation 18; 590 mg; 1.53 mmol), hydroxylamine hydrochloride (637 mg; 9.16 mmol) (769 mg; 9.16 mmol) followed by ethanol (15 ml) and the resulting suspension was stirred at 80° C. overnight. More hydroxylamine hydrochloride and sodium bicarbonate (3 equivalents of each) were added and the mixture stirred at 80° C. for ca. 14 h. The mixture was cooled to room temperature, and the precipitate was filtered off and the residue washed with ethanol. The combined filtrate and washings were evaporated in vacuo and the residue partitioned between water and ether. The phases were separated and the aqueous phase extracted twice with ether. The combined organic phases were dried over MgSO4 and concentrated in vacuo to give the title compound (547 mg).

後処理

  1. stirringthe mixture stirred at 80° C. for ca. 14 h
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationthe precipitate was filtered off
  4. washthe residue washed with ethanol
  5. customThe combined filtrate and washings were evaporated in vacuo
  6. customthe residue partitioned between water and ether
  7. customThe phases were separated
  8. extractionthe aqueous phase extracted twice with ether
  9. dry with materialThe combined organic phases were dried over MgSO4
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-999670fbf3634ff79d7b6edd0196aada
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263620B2

反応ノート

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