Sodium Hydroxide → HCID 23469722, 화합물

HRID 128464

반응식

HRID 128464 반응식
Cl.[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].[OH-].[Na+].CN([CH:16]=[N:17][C:18](=O)[C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)C>O.O1CCOCC1.C(O)(=O)C>[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:18]([C:19]2[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=2)=[N:17][CH:16]=[N:10]1

참가 물질

7

반응물 3

HCID 14798Sodium HydroxideHCID 2723910Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1)HCID 12550338HCID 12550338, 화합물

생성물 1

HCID 23469722HCID 23469722, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매2회HCID 312751,4-Dioxane용매2회

실험 절차

A 25.0 g. portion of o-fluorophenylhydrazine hydrochloride is dissolved in 150 ml. of p-dioxane with warming and 31.0 ml. of 5 N sodium hydroxide is added. After solution is complete, 80 ml. of glacial acetic acid and 210 ml. of water are added followed by 28.1 g. of N-(dimethylaminomethylene)-p-nitrobenzamide in 100 ml. of warm p-dioxane. This reaction mixture is heated at 90°-95° C. for 1.5 hours, then cooled and poured into 1500 ml. of water. The solid is collected by filtration, washed with water, dried and crystallized from 200 ml. of ethanol, giving 13.9 g. of the desired product as a tan solid, mp. 143°-145° C.

후처리

  1. temperatureThis reaction mixture is heated at 90°-95° C. for 1.5 hours
  2. temperaturecooled
  3. additionpoured into 1500 ml
  4. filtrationThe solid is collected by filtration
  5. washwashed with water
  6. customdried
  7. customcrystallized from 200 ml
  8. customof ethanol, giving 13.9 g

출처 및 근거

ORD 기록
ord-769e086f96e04461b8f8105605192835
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259504

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