Hydrochloric Acid → HCID 136066331, 화합물

HRID 236282노트

반응식

HRID 236282 반응식
CS[C:3]1[NH:12][C:11](=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=1.[CH3:14][O:15][CH2:16][CH2:17][O:18][C:19]1[CH:20]=[N:21][NH:22][CH:23]=1.O.Cl>CN(C)C=O>[CH3:14][O:15][CH2:16][CH2:17][O:18][C:19]1[CH:20]=[N:21][N:22]([C:3]2[NH:12][C:11](=[O:13])[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[N:4]=2)[CH:23]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 135633474-(2-Methoxyethoxy)-1H-pyrazoleHCID 1354271042-(Methylsulfanyl)quinazolin-4(1H)-one

생성물 1

HCID 136066331HCID 136066331, 화합물수율 58.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

96 g (0.5 mole) of 2-methylthio-4(3H)-quinazolinone are stirred in 250 ml of dimethylformamide with 142 g (1 mole) of 4-(β-methoxy-ethoxy)pyrazole at the reflux temperature for 40 hours. After cooling, 2.5 litres of water are added and a pH value of 3 is established with hydrochloric acid. The crude product which separates out (97.3 g of melting point 119°-24°) is recrystallized from isopropanol. 83.8 g of 2-(4-β-methoxyethoxy-1H-pyrazol-1-yl)-4(3H)-quinazolinone of melting point 125° to 127° C. are obtained.

후처리

  1. temperatureAfter cooling
  2. customis recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-907e8ea32f5841feb1027446b48fdfae
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04644000

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