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

HRID 488065

反応式

HRID 488065 の反応式
[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

参加物

9

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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)].

後処理

  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

出典と根拠

ORDレコード
ord-c5e8126c74af475bbb87348101a348c0
出典データセット
uspto-grants-1994_03
特許番号
US05298632

関連ノート

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