Salicylic Acid → HCID 68880764、化合物

HRID 1166193

反応式

HRID 1166193 の反応式
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].Cl[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH2:19][Cl:20])[N:14]=1.[CH2:21]([O:23]CC)[CH3:22]>CN(C=O)C>[Cl:20][CH2:19][C:15]1[N:14]=[C:13]([CH3:12])[C:18]([O:9][C:1](=[O:10])[C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4][C:21](=[O:23])[CH3:22])=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 338Salicylic AcidHCID 3283Diethyl EtherHCID 3166542,6-Bis(chloromethyl)pyridine

生成物 1

HCID 68880764HCID 68880764、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of salicylic acid (1.6 g, 8.88 mmoles) in N,N′-dimethylformamide (20 ml) and under stirring sodium ethylate (0.64 g, 8.88 mmoles) is added. After 30 minutes the obtained solution is added to a solution of 2,6-bis-(chloromethyl)pyridine (4.72 g, 26.81 mmoles) in N,N′-dimethylformamide (20 ml). The solution is left at room temperature for 7 days, under stirring, then is diluted with ethyl ether and washed with water. The separated organic phases are anhydrified with sodium sulphate and the solvent is evaporated at reduced pressure. The reaction crude product is purified by chromatography on silica gel by eluting with n-hexane/ethyl acetate 7/3. 1.7 g of the product as yellow oil are obtained.

後処理

  1. washwashed with water
  2. customthe solvent is evaporated at reduced pressure
  3. customThe reaction crude product
  4. customis purified by chromatography on silica gel
  5. washby eluting with n-hexane/ethyl acetate 7/3

出典と根拠

ORDレコード
ord-b05a90314d204242a2ac14f8fc776bbd
出典データセット
uspto-grants-2003_09
特許番号
US06613784B1

関連ノート

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