Phosphoric Acid → HCID 178433533, compound

HRID 1734760Notes

Reaction equation

HRID 1734760 reaction equation
[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

Participants

4

Reactant 2

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

Product 1

HCID 178433533HCID 178433533, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
20 °C

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-1a6ed67652544649b5f4c2cce7403a1c
Source dataset
uspto-grants-1996_07
Patent number
US05534644

Reaction notes

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