Pyridine → HCID 19828473、化合物

HRID 1494524ノート

反応式

HRID 1494524 の反応式
[CH3:1][C:2]1([CH3:22])[O:7][CH2:6][C:5]2[C:8]([CH:13](O)[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1.N1C=CC=CC=1.S(Cl)([Cl:31])=O>C(Cl)Cl>[CH3:1][C:2]1([CH3:22])[O:7][CH2:6][C:5]2[C:8]([CH:13]([Cl:31])[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1

参加物

5

反応物 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 11529834(4-chlorophenyl)-(2,2,8-trimethyl-4H-[1,3]dioxino[4,5-c]pyridin-5-yl)methanol

生成物 1

HCID 19828473HCID 19828473、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

88 mg (0.275 mmole) of (+)-2,2,8-trimethyl-5-(4-chloro-α-hydroxybenzyl)-pyrido-[4,3-e]-1,3-dioxane are poured into a 5 ml flask, dissolved in 1 ml of methylene chloride and the flask is sealed under an atmosphere of nitrogen. 22 μl (0.27 mmole) of anhydrous pyridine are injected via a glass syringe. 36 μl (0.54 mmole) of thionyl chloride are then added dropwise. At disappearance (2 hours later) of the starting material (checked by TLC), the solvent is evaporated off under reduced pressure.

後処理

  1. customthe flask is sealed under an atmosphere of nitrogen
  2. customAt disappearance (2 hours later) of the starting material (checked by TLC), the solvent is evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-475ca8ea1e1a4280a2598f4fd0196dd1
出典データセット
uspto-grants-1991_06
特許番号
US05026855

反応ノート

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