1,3-Propanediamine → Drometrizole

HRID 27259

반응식

HRID 27259 반응식
NCCCN.O.[N+:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N:16]=[N:17][C:18]1[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][C:19]=1[OH:25])([O-])=O>C1(C)C(C)=CC=CC=1.[Cu].II.CC(O)=O>[OH:25][C:19]1[CH:20]=[CH:21][C:22]([CH3:24])=[CH:23][C:18]=1[N:17]1[N:16]=[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]2=[N:7]1

참가 물질

6

반응물 3

HCID 4281,3-PropanediamineHCID 962WaterHCID 740294-Methyl-2-[2-(2-nitrophenyl)diazenyl]phenol

생성물 1

HCID 17113Drometrizole

시약·촉매·용매 2

HCID 131711869copper II-acetate촉매HCID 7237O-Xylene용매

실험 절차

11.6 g of 1,3-diaminopropane (0.16 mol) and 2 g of copper-II-acetate (0.01 mol) are placed into 50 ml of water and the whole is heated, with the exclusion of air and with stirring, to 85°-90° C. A solution of 10 g of 2-nitro-2'-hydroxy-5'-methyl-azobenzene (0.04 mol) in 100 ml of xylene heated to 60° C. is then added, and after 20 hours the reaction mixture is cooled to room temperature. The aqueous phase is separated, and the organic phase is extracted with aqueous hydrochloric acid, and then washed with water until neutral. The xylene is distilled off to leave 7.7 g of crude product. Analysis of the crude product by means of LC (liquid chromatography) gives 86% of theory of 2-(2'-hydroxy-5'-methylphenyl)-benzotriazole.

후처리

  1. temperaturethe whole is heated, with the exclusion of air
  2. additionis then added
  3. customThe aqueous phase is separated
  4. extractionthe organic phase is extracted with aqueous hydrochloric acid
  5. washwashed with water until neutral
  6. distillationThe xylene is distilled off
  7. customto leave 7.7 g of crude product

출처 및 근거

ORD 기록
ord-8705d867eebf45b3a038ae1dfffdf136
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220788

연결된 노트

불러오는 중…