Water → 5-[(Hydroxyimino)methyl]-3-thiophenecarbonitrile

HRID 1582900ノート

反応式

HRID 1582900 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=O)[S:6][CH:7]=1)#[N:2].C(=O)([O-])[O-].[Na+].[Na+].Cl.[NH2:17][OH:18].O>CO>[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[N:17][OH:18])[S:6][CH:7]=1)#[N:2]

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 122800095-Formylthiophene-3-carbonitrile

生成物 1

HCID 738516325-[(Hydroxyimino)methyl]-3-thiophenecarbonitrile収率 97.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
10 °C

実験手順

11.6 g (84.6 mmol) of 4-cyanothiophene-2-carbaldehyde were dissolved in 140 ml of methanol and 12.3 g (116.1 mmol) of sodium carbonate were added. 6.5 [lacuna] (93.5 mmol) of hydroxylamine hydrochloride were subsequently added at 15° C. with cooling, a little at a time, and the mixture was stirred for 2 hours at 10° C. After 80 ml of water had been added, the reaction mixture was extracted five times using in each case 50 ml of diethyl ether, the organic phase was dried over sodium sulfate and the solvent was removed in vacuo. 12.5 g of the required product resulted as a yellow crystal powder (96% of theory).

後処理

  1. temperaturewith cooling
  2. extractionthe reaction mixture was extracted five times
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-428f6cf68ce44ccd90b0424d6b713a43
出典データセット
uspto-grants-2004_05
特許番号
US06740647B1

反応ノート

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