Phosphoric Acid → HCID 178433533、化合物

HRID 265640ノート

反応式

HRID 265640 の反応式
[S:1]([CH:4]([CH2:8][CH2:9][Cl:10])[C:5](=O)[CH3:6])[C:2]#[N:3].P(=O)(O)(O)[OH:12]>O>[OH:12][C:2]1[S:1][C:4]([CH2:8][CH2:9][Cl:10])=[C:5]([CH3:6])[N:3]=1

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 108776933-Thiocyanato-5-chloro-2-pentanone

生成物 1

HCID 178433533HCID 178433533、化合物収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
20 °C

実験手順

355,3 g (2 moles) of distilled 3-thiocyanato-5-chloro-2-pentanone are added into 360 cm3 of 85% phosphoric acid under stirring. The temperature of the reaction mixture is increased to 95° C. in water bath within about 1 hour and then it is stirred for half and hour between 95° to 100° C. The brown solution is cooled to 20° C. and poured into 660 cm3 of water. The precipitated beige crystals are removed by suction after a stirring for half an hour, washed neutral with water and dried in vacuo at a temperature of 60° C. 337 g (95%) of pale beige 2-hydroxy-4-methyl-5-(2-chloroethyl)thiazole are obtained, m.p.: 151°-152° C. After recrystallization from benzene the melting point is 157°-158° C.

後処理

  1. stirringit is stirred for half and hour between 95° to 100° C
  2. customThe precipitated beige crystals are removed by suction after a stirring for half an hour
  3. washwashed neutral with water
  4. customdried in vacuo at a temperature of 60° C

出典と根拠

ORDレコード
ord-f691c69bdd404e6ba373b0e0ae6a908a
出典データセット
uspto-grants-1997_07
特許番号
US05648498

反応ノート

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