1,2-Dimethoxyethane → HCID 11459000、化合物

HRID 2163196ノート

反応式

HRID 2163196 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1.[OH-].[K+].C(COC)OC>O.CN(C)P(N(C)C)(N(C)C)=O>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([O:17][C:14]2[CH:15]=[CH:16][C:11]([O:10][CH3:9])=[CH:12][CH:13]=2)[N:3]=1

参加物

7

反応物 4

HCID 80711,2-DimethoxyethaneHCID 90154-MethoxyphenolHCID 14797Potassium HydroxideHCID 169892,6-Dichloropyridine

生成物 1

HCID 11459000HCID 11459000、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 12679Hexamethylphosphoramide溶媒

実験手順

A solution comprising 14.8 grams (0.1 mole) of 2,6-dichloropyridine, 12.4 grams (0.1 mole) of 4-methoxyphenol and 8.4 grams (0.15 mole) of flake potassium hydroxide in 100 milliliters of a 1:1 mixture of monoglyme and hexamethylphosphoramide was stirred for 24 hours at room temperature. The resulting mixture was diluted with water and thoroughly extracted with hexane. The extract was washed with water, dried and concentrated under reduced pressure. The residue was recrystallized from pentane giving 14.5 grams (64 percent of theoretical) of 2-chloro-6-(4-methoxyphenoxy)pyridine which melted at 63°-65° C.

後処理

  1. extractionthoroughly extracted with hexane
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from pentane giving 14.5 grams (64 percent of theoretical) of 2-chloro-6-(4-methoxyphenoxy)pyridine which melted at 63°-65° C.

出典と根拠

ORDレコード
ord-0a5fe9ba39a5445fa67a3a082a64c74a
出典データセット
uspto-grants-1979_01
特許番号
US04132783

反応ノート

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