Pyridine → HCID 86742998、化合物

HRID 1761772ノート

反応式

HRID 1761772 の反応式
[OH:1][CH2:2]/[CH:3]=[C:4](/[CH3:23])\[CH2:5][CH2:6]/[CH:7]=[C:8](\[CH3:22])/[CH2:9][CH2:10][C:11](=[O:21])[CH:12]([CH3:20])[CH2:13][S:14][CH2:15][C:16]([O:18][CH3:19])=[O:17].N1C=CC=CC=1.[C:30](OC(=O)C)(=[O:32])[CH3:31]>C(Cl)Cl>[C:30]([O:1][CH2:2]/[CH:3]=[C:4](/[CH3:23])\[CH2:5][CH2:6]/[CH:7]=[C:8](\[CH3:22])/[CH2:9][CH2:10][C:11](=[O:21])[CH:12]([CH3:20])[CH2:13][S:14][CH2:15][C:16]([O:18][CH3:19])=[O:17])(=[O:32])[CH3:31]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 86742997HCID 86742997、化合物

生成物 1

HCID 86742998HCID 86742998、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 300 mg (0.00088 mol) of methyl [[(6E, 10Z)-12-hydroxy-2,6,10-trimethyl-3-oxo-6,10-dodecadienyl]thio]acetate in 5 ml of methylene chloride is treated with 0.5 ml of pyridine and 0.4 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 solvent each time on a rotary evaporator. The residue is chromatographed on silica gel with ether. There is obtained (2Z,6E)-12-[[(methoxycarbonyl)methyl]thio]-3,7,11-trimethyl-10-oxo-2,6-dodecadienyl acetate which exhibits the following bands in the IR spectrum: 1710 cm-1, 1657 cm-1, 1552 cm-1, 1445 cm-1, 1375 cm-1, 1290 cm-1, 1235 cm-1.

後処理

  1. customAfter removing the solvent the residue
  2. customon a rotary evaporator
  3. customThe residue is chromatographed on silica gel with ether

出典と根拠

ORDレコード
ord-1383ff6f97684a92ab8437ce2e945f52
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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