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

Phosphorus pentachloride → 2-(4-Methyl-1-piperazinyl)-5-nitrobenzoxazole

HRID 1636862
노트
인쇄 미리보기

반응식

HRID 1636862 반응식
P(Cl)(Cl)(Cl)(Cl)Cl.S[C:8]1[O:9][C:10]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:11]=2[N:12]=1.[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C1(C)C=CC=CC=1>[CH3:20][N:21]1[CH2:26][CH2:25][N:24]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:11]=3[N:12]=2)[CH2:23][CH2:22]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24819Phosphorus pentachlorideHCID 531671-MethylpiperazineHCID 178526504HCID 178526504, 화합물

생성물 1

HCID 225581882-(4-Methyl-1-piperazinyl)-5-nitrobenzoxazole

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

Phosphorus pentachloride (1.37 g) was dissolved in anhydrous toluene (18 ml), the resulting solution was mixed with 2-mercapto-5-nitrobenzoxazole (900 mg) which has been obtained in the same manner as described in Reference Example 1, and the mixture was then stirred with heating at 100° C. for 3 hours. With cooling in an ice bath, to this was added dropwise N-methylpiperazine (6.09 ml). After 20 minutes of stirring, the thus obtained mixture was extracted with ethyl acetate, and the organic layer was washed with saturated sodium bicarbonate aqueous solution and saturated brine in that order. After drying with magnesium sulfate, the solvent was evaporated under a reduced pressure, and the resulting residue was purified by a silica gel column chromatography (methylene chloride:methanol=10:1) to obtain 2-(4-methyl-1-piperazinyl)-5-nitrobenzoxazole (56.1 mg) in the form of yellow crystalline powder.

후처리

  1. customhas been obtained in the same manner
  2. temperatureWith cooling in an ice bath
  3. stirringAfter 20 minutes of stirring
  4. extractionthe thus obtained mixture was extracted with ethyl acetate
  5. washthe organic layer was washed with saturated sodium bicarbonate aqueous solution and saturated brine in that order
  6. dry with materialAfter drying with magnesium sulfate
  7. customthe solvent was evaporated under a reduced pressure
  8. customthe resulting residue was purified by a silica gel column chromatography (methylene chloride:methanol=10:1)

출처 및 근거

ORD 기록
ord-7f7d30d016184a568f1a89b2d05a73c6
출처 데이터셋
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06037342

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트