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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dichloromethane → 5-(4-chlorophenyl)-4-(2,4-dichlorophenyl)-2-oxo-4-(1H-1,2,4-triazol-1-yl)methyl-1,3-dioxolane

HRID 65025
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인쇄 미리보기

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HRID 65025 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:25])[C:9]([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=2[Cl:24])([OH:16])[CH2:10][N:11]2[CH:15]=[N:14][CH:13]=[N:12]2)=[CH:4][CH:3]=1.[C:26](Cl)(=O)[O:27]C1C=CC=CC=1.C(=O)([O-])O.[Na+].C(Cl)Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[O:25][C:26](=[O:27])[O:16][C:9]2([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=2[Cl:24])[CH2:10][N:11]2[CH:15]=[N:14][CH:13]=[N:12]2)=[CH:4][CH:3]=1
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참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 15891Phenyl chloroformateHCID 516892Sodium BicarbonateHCID 13777825HCID 13777825, 화합물

생성물 1

HCID 137270005-(4-chlorophenyl)-4-(2,4-dichlorophenyl)-2-oxo-4-(1H-1,2,4-triazol-1-yl)methyl-1,3-dioxolane수율 87.5%

시약·촉매·용매 1

HCID 1049
Pyridine
용매

실험 절차

To a solution of 500 mg of 1-(4-chlorophenyl)-2-(2,4-dichlorophenyl)-3-(1H-1,2,4-triazol-1-yl)-1,2-propanediol in 1 ml of dry pyridine is added 300 mg of phenyl chlorocarbonate, and the resultant mixture is allowed to react at room temperature for 18 hours. The reaction mixture is mixed with aqueous sodium hydrogencarbonate solution and shaken with methylene chloride. The organic layer is washed with water, dried over anhydrous sodium sulfate and concentrated. The residue is chromatographed on a column of silica-gel, which is eluted with 2% methanolmethylene chloride. The eluate is concentrated and the residue is crystallized from ethyl acetate-isopropyl ether to give 466 mg of 5-(4-chlorophenyl)-4-(2,4-dichlorophenyl)-2-oxo-4-(1H-1,2,4-triazol-1-yl)methyl-1,3-dioxolane as crystals melting at 178° to 179° C. The yield is 87%.

후처리

  1. customto react at room temperature for 18 hours
  2. washThe organic layer is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue is chromatographed on a column of silica-gel, which
  6. washis eluted with 2% methanolmethylene chloride
  7. concentrationThe eluate is concentrated
  8. customthe residue is crystallized from ethyl acetate-isopropyl ether

출처 및 근거

ORD 기록
ord-032c252c1d5a4fc1aa0d031bd1dc3929
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04612322

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