Hydrochloric Acid → Tetrahydrofurfuryl 2-(4,6-dimethoxypyrimidin-2-yl)oxybenzoate

HRID 488065

반응식

HRID 488065 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=2[C:14]([OH:16])=[O:15])[N:4]=1.[O:21]1[CH2:25][CH2:24][CH2:23][CH:22]1O.[CH:27](C1C=C(C(C)C)C=C(C(C)C)C=1S(Cl)(=O)=O)(C)C.CN1C=CN=C1.Cl>O1CCCC1.C(Cl)(Cl)Cl.C(OCC)(=O)C>[CH3:10][O:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([O:11][C:12]2[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=2[C:14]([O:16][CH2:27][CH:22]2[O:21][CH2:25][CH2:24][CH2:23]2)=[O:15])[N:6]=1

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 13901-MethylimidazoleHCID 810422,4,6-Tris(1-methylethyl)benzenesulfonyl chlorideHCID 93002Tetrahydro-2-hydroxyfuranHCID 1841852-((4,6-Dimethoxypyrimidin-2-yl)oxy)benzoic acid

생성물 1

HCID 15278238Tetrahydrofurfuryl 2-(4,6-dimethoxypyrimidin-2-yl)oxybenzoate

시약·촉매·용매 3

HCID 6212Chloroform용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

0.55 Gram of 2-(4,6-dimethoxypyrimidin-2-yl)oxybenzoic acid, 0.21 g of tetrahydrofuryl alcohol and 0.85 g of 2,4,6-triisopropylbenzenesulfonyl chloride were dissolved in 5 ml of tetrahydrofuran. Subsequently, 0.45 g of 1-methylimidazole was added to the mixture. After stirring the resulting solution at room temperature for 1 hour in order to carry out the reaction, the reaction solution was poured into diluted hydrochloric acid, and exracted with ethyl acetate. The organic layer separated from the aqueous layer was washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue obtained was subjected to silica gel column chromatography (mfd. by Merch & Co., Inc., solvent: chloroform) to obtain 0.30 g of tetrahydrofurfuryl 2-(4,6-dimethoxypyrimidin-2-yl)oxybenzoate [present compound (III-9)].

후처리

  1. customthe reaction
  2. customThe organic layer separated from the aqueous layer
  3. washwas washed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue obtained

출처 및 근거

ORD 기록
ord-c5e8126c74af475bbb87348101a348c0
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05298632

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