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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Pyridine → HCID 67600187, 화합물

HRID 1417331
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HRID 1417331 반응식
[N:1]1([C:6]2[CH:17]=[CH:16][C:9]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][NH2:15])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.N1C=CC=CC=1.[CH3:24][O:25][C:26]1[CH:34]=[CH:33][C:29]([C:30](Cl)=[O:31])=[CH:28][CH:27]=1>ClCCl>[CH3:24][O:25][C:26]1[CH:34]=[CH:33][C:29]([C:30]([NH:15][CH2:14][CH2:13][CH2:12][CH2:11][O:10][C:9]2[CH:16]=[CH:17][C:6]([N:1]3[CH:5]=[CH:4][N:3]=[CH:2]3)=[CH:7][CH:8]=2)=[O:31])=[CH:28][CH:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7477p-Anisoyl chlorideHCID 10922371HCID 10922371, 화합물

생성물 1

HCID 67600187HCID 67600187, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-10 °C

실험 절차

A solution of 2.3 g of 4-[4-(1H-imidazol-1-yl)phenoxy]butaneamine (Example 2) in 50 ml of dichloromethane containing 2 ml of pyridine is treated with 2.0 g of 4-methoxybenzoyl chloride. The reaction mixture is allowed to stand at room temperature for 18 hours, and is then heated at reflux for one hour. The volatiles are removed in vacuo. The residue is partitioned between 100 ml of dichloromethane and 100 ml of water. The dichloromethane layer is dried over Na2SO4, and then heated to gentle boiling. Hexane is then added to turbidity and the mixture cooled at -10° C. A tacky precipitate results and crystals develop in the supernatant solvent. These are collected, washed with hexane, and dried in vacuo at room temperature; m.p. 125°-126° C.; yield, 0.4 g.

후처리

  1. temperatureis then heated
  2. temperatureat reflux for one hour
  3. customThe volatiles are removed in vacuo
  4. customThe residue is partitioned between 100 ml of dichloromethane and 100 ml of water
  5. dry with materialThe dichloromethane layer is dried over Na2SO4
  6. temperatureheated to gentle boiling
  7. additionHexane is then added to turbidity
  8. customA tacky precipitate results
  9. customThese are collected
  10. washwashed with hexane
  11. customdried in vacuo at room temperature
  12. customyield

출처 및 근거

ORD 기록
ord-9b4a9f8b3f7443d8a06676047733f240
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05877196

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