Pyridine → HCID 86742986、化合物

HRID 1761754ノート

反応式

HRID 1761754 の反応式
[OH:1][CH2:2]/[CH:3]=[C:4](/[CH3:17])\[CH2:5][CH2:6]/[CH:7]=[C:8](\[CH3:16])/[CH2:9][CH2:10][C:11](=[O:15])[C:12]([CH3:14])=[CH2:13].N1C=CC=CC=1.[C:24](OC(=O)C)(=[O:26])[CH3:25]>C(Cl)Cl>[C:24]([O:1][CH2:2]/[CH:3]=[C:4](/[CH3:17])\[CH2:5][CH2:6]/[CH:7]=[C:8](\[CH3:16])/[CH2:9][CH2:10][C:11](=[O:15])[C:12]([CH3:14])=[CH2:13])(=[O:26])[CH3:25]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 86742985HCID 86742985、化合物

生成物 1

HCID 86742986HCID 86742986、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 0.5 g (0.0021 mol) of (6E,10Z)-12-hydroxy-2,6,10-trimethyl-1,6,10-dodecatrien-3-one dissolved in 5 ml of methylene chloride and 1.3 ml of pyridine is treated with 1 ml of acetic anhydride. The solution is stirred at room temperature for 18 hours under argon. After removing the solvent the residue is taken up three times in toluene and freed from the solvent on a rotary evaporator. The residue is chromatographed on silica gel with ether-hexane 1:5. There is obtained (2Z,6E)-3,7,11-trimethyl-10-oxo-2,6,11-dodecatrienyl acetate which has the following bands in the IR spectrum: 1735 cm-1, 1677 cm-1, 1630 cm-1, 1448 cm-1, 1368 cm-1, 950 cm-1.

後処理

  1. customAfter removing the solvent the residue
  2. customfreed from the solvent on a rotary evaporator
  3. customThe residue is chromatographed on silica gel with ether-hexane 1:5

出典と根拠

ORDレコード
ord-28b5c8f07fc34bda9699c6cc492a5bca
出典データセット
uspto-grants-1989_05
特許番号
US04827004

反応ノート

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