Hydrochloric Acid → HCID 19600266、化合物

HRID 611256ノート

反応式

HRID 611256 の反応式
[C:1]([C:9]1[CH:29]=[CH:28][C:12]([C:13]([N:15]2[CH2:20][CH2:19][C:18]3[CH:21]=[C:22]([C:24]([O:26]C)=[O:25])[O:23][C:17]=3[CH2:16]2)=[O:14])=[CH:11][CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O1CCCC1.[OH-].[Na+]>[C:1]([C:9]1[CH:10]=[CH:11][C:12]([C:13]([N:15]2[CH2:20][CH2:19][C:18]3[CH:21]=[C:22]([C:24]([OH:26])=[O:25])[O:23][C:17]=3[CH2:16]2)=[O:14])=[CH:28][CH:29]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 19600240HCID 19600240、化合物

生成物 1

HCID 19600266HCID 19600266、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

To a solution of 126 mg (0.324 mmol) of methyl 6-(4-benzoylbenzoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine-2-carboxylate in 10 ml of tetrahydrofuran, 1 ml of 2 N aqueous sodium hydroxide was added, followed by stirring at room temperature for 1 day. The reaction mixture was acidified with 10 ml of 1 N hydrochloric acid and extracted with diethyl ether 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (ethyl acetate/methanol=4/1 to chloroform/methanol=1/1) to yield the desired product.

後処理

  1. extractionextracted with diethyl ether 3 times
  2. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe resulting crude product was purified by silica gel column chromatography (ethyl acetate/methanol=4/1 to chloroform/methanol=1/1)

出典と根拠

ORDレコード
ord-3d4203d0a7e94fc0b05be808b7d77e36
出典データセット
uspto-grants-1999_12
特許番号
US05998433

反応ノート

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