Phosphoric Acid → HCID 178433533, 화합물

HRID 265640노트

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HRID 265640 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178433533HCID 178433533, 화합물수율 95%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f691c69bdd404e6ba373b0e0ae6a908a
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648498

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