Sodium hydride → HCID 14878964、化合物

HRID 1084770ノート

反応式

HRID 1084770 の反応式
[H-].[Na+].Cl[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:6]=1.[Cl:18][CH2:19][C:20]([CH3:24])([CH3:23])[CH2:21][OH:22]>CN(C=O)C>[Cl:18][CH2:19][C:20]([CH3:24])([CH3:23])[CH2:21][O:22][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:6]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 834071-Propanol, 3-chloro-2,2-dimethyl-HCID 138492412-Chloromethyl-6-phenoxypyridine

生成物 1

HCID 14878964HCID 14878964、化合物収率 11.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Under a nitrogen atmosphere, 0.65 g of sodium hydride (60% oily suspension) was suspended in 10 ml of dry DMF, and a solution of 3.23 g of 2-chloromethyl-6-phenoxypyridine and 2.00 g of 3-chloro-2,2-dimethylpropanol in 10 ml of dry DMF was added dropwise with ice-cooling. After stirring for 12 hours at room temperature, the reaction solution was poured into dilute hydrochloric acid-ice water and extracted twice with diethyl ether. The ether layers were combined, washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was subjected to column chromatography on silica gel (developing solvent, hexane : ethyl acetate=50:1) to obtain 0.52 g of desired 6-phenoxy-2-pyridylmethyl 3-chloro-2,2-dimethylpropyl ether [present compound (1)] as a colorless oily product.

後処理

  1. temperaturecooling
  2. extractionextracted twice with diethyl ether
  3. washwashed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-8c97893830aa40ed90674fb2ab25535d
出典データセット
uspto-grants-1991_04
特許番号
US05006538

反応ノート

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