Ethanol → HCID 178496020、化合物

HRID 909910ノート

反応式

HRID 909910 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][CH:28]=1)[CH2:6][CH2:7][O:8][CH2:9][CH2:10][C:11]([N:13]([CH:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1)[CH2:14][CH:15]([O:18][CH3:19])[O:16][CH3:17])=[O:12])#[N:2].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:36][OH:37].C(O)C>O>[CH:20]1([N:13]([CH2:14][CH:15]([O:18][CH3:19])[O:16][CH3:17])[C:11](=[O:12])[CH2:10][CH2:9][O:8][CH2:7][CH2:6][C:5]2[CH:26]=[CH:27][CH:28]=[C:3]([C:1](=[NH:2])[NH:36][OH:37])[CH:4]=2)[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1

参加物

6

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 581685553-(3-Cyanophenethoxy)-N-cyclohexyl-N-(2,2-dimethoxyethyl)propanamide

生成物 1

HCID 178496020HCID 178496020、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
90 °C

実験手順

To 3-(3-cyanophenethoxy)-N-cyclohexyl-N-(2,2-dimethoxyethyl)propanamide [Example 10, Step i)] (1.5 g) within a 35 mL microwave vial was added potassium carbonate (0.80 g), hydroxylamine hydrochloride (0.402 g), water (2.5 mL) and ethanol (10 mL). The vial was sealed and stirred for 3 days before being heated at 90° C. for a total of 3 h. The reaction was diluted with water, extracted twice with ethyl acetate, which was pooled and washed twice with water, twice with brine, dried over sodium sulphate, filtered and the solvent removed to afford a colourless gum (1.7 g). This material was used in the next step directly.

後処理

  1. customThe vial was sealed
  2. extractionextracted twice with ethyl acetate, which
  3. washwashed twice with water, twice with brine
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent removed

出典と根拠

ORDレコード
ord-29daa0823a604a05b6700d27bb8df2ec
出典データセット
uspto-grants-2011_09
特許番号
US08017602B2

反応ノート

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