Salicylic Acid → HCID 68880764, 화합물

HRID 1166193

반응식

HRID 1166193 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 68880764HCID 68880764, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b05a90314d204242a2ac14f8fc776bbd
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06613784B1

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