Water → 1-(5-Methylthiophen-3-yl)ethan-1-one

HRID 2420251ノート

反応式

HRID 2420251 の反応式
[CH3:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([OH:9])=O)[CH:6]=1.[CH2:10](OCC)C.C[Li].O>C(O)C>[CH3:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([CH3:10])=[O:9])[CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 3283Diethyl EtherHCID 2090693-Thiophenecarboxylic acid, 5-methyl-HCID 178418348HCID 178418348、化合物

生成物 1

HCID 212902951-(5-Methylthiophen-3-yl)ethan-1-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

2-Methylthiophene-4-carboxylic acid (14.2 g., 0.1 mole) prepared by the method of Shvedov et al., Khim. Geterotsikl. Soedin. 1010 (1967); Chem. Abstrs., 69, 51922j (1968) in 250 ml. of ethyl ether is cooled to -10° to 0° C. and an ethereal solution of methyl lithium (4.4 g., 0.2 mole) is added dropwise while maintaining the reaction mixture below 0° C. After stirring for 1 hour at 0° C., a solution of 4 g. of water in 100 ml. of ethanol is added cautiously and the mixture allowed to warm to room temperature. The desired product is then isolated by partitioning the reaction mixture between ether and water and evaporation of the organic extracts.

後処理

  1. temperaturewhile maintaining the reaction mixture below 0° C
  2. temperatureto warm to room temperature

出典と根拠

ORDレコード
ord-2fc3fbe0f80e47b0b95fb786b72ffbff
出典データセット
uspto-grants-1978_08
特許番号
US04110342

反応ノート

読み込み中…