홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1-Chloro-4-nitrobenzene → 1-Methyl-4-(4-nitrophenoxy)-3,5-diphenyl-1H-pyrazole

HRID 436611
노트
인쇄 미리보기

반응식

HRID 436611 반응식
[OH:1][C:2]1[C:3]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:4][N:5]([CH3:13])[C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.CC(C)([O-])C.[K+].Cl[C:27]1[CH:32]=[CH:31][C:30]([N+:33]([O-:35])=[O:34])=[CH:29][CH:28]=1.[OH-].[Na+]>O.CN(C=O)C>[CH3:13][N:5]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[C:2]([O:1][C:27]2[CH:32]=[CH:31][C:30]([N+:33]([O-:35])=[O:34])=[CH:29][CH:28]=2)[C:3]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[N:4]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 74741-Chloro-4-nitrobenzeneHCID 14798Sodium HydroxideHCID 12326421HCID 12326421, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 213980591-Methyl-4-(4-nitrophenoxy)-3,5-diphenyl-1H-pyrazole수율 91.4%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A solution of 4-hydroxy-1-methyl-3,5-diphenylpyrazole (10 g, 0.04 mole), potassium t-butoxide (4.5, 0.04 mole) and dry DMF (150 ml) is stirred and heated to 60° C. The green fluorescent solution is cooled to room temperature and p-chloronitrobenzene (6.0 g, 0.038 mole) is added. The dark green solution is heated at 60° C for 24 hours and then poured into water, made alkaline with 1N sodium hydroxide and extracted with ether. The ether layer is separated, washed well with water, dried and stripped in vacuo to give a bright yellow solid 12.9 g (86.5%), m.p. 85° C to 110° C. The solid is chromatographed on silica gel with benzene to give a yellow crystalline solid 11.3 g, m.p. 74° C to 100° C. Recrystallization from methanol (185 ml) affords white crystals 5.5 g (37%) m.p. 120° C to 122° C.

후처리

  1. temperatureThe green fluorescent solution is cooled to room temperature
  2. temperatureThe dark green solution is heated at 60° C for 24 hours
  3. extractionextracted with ether
  4. customThe ether layer is separated
  5. washwashed well with water
  6. customdried

출처 및 근거

ORD 기록
ord-4f62de5c20db4953a164c0d4ada95afe
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04009277

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트