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Acetic Acid → Ethyl 6-(4-fluorobenzyl)-4-methoxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridine-1-carboxylate

HRID 1817302
ノート
印刷プレビュー

反応式

HRID 1817302 の反応式
CO.[CH3:3][Si](C=[N+]=[N-])(C)C.[F:10][C:11]1[CH:34]=[CH:33][C:14]([CH2:15][N:16]2[CH2:25][CH2:24][C:23]3[C:22]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[N:21][CH:20]=[C:19]([OH:31])[C:18]=3[C:17]2=[O:32])=[CH:13][CH:12]=1.C(O)(=O)C>C(Cl)(Cl)Cl>[F:10][C:11]1[CH:34]=[CH:33][C:14]([CH2:15][N:16]2[CH2:25][CH2:24][C:23]3[C:22]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[N:21][CH:20]=[C:19]([O:31][CH3:3])[C:18]=3[C:17]2=[O:32])=[CH:13][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 887Methanol2 回HCID 167693Trimethylsilyldiazomethane2 回HCID 69061030Ethyl 6-(4-fluorobenzyl)-4-hydroxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridine-1-carboxylate

生成物 1

HCID 69058090Ethyl 6-(4-fluorobenzyl)-4-methoxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of chloroform (10 mL) and methanol (10 mL) was added trimethylsilyl diazomethane (2.0 M in hexanes, 5 mL, 0.01 mole). After stirring for 10 minutes at room temperature, ethyl 6-(4-fluorobenzyl)-4-hydroxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridine-1-carboxylate (1.6 g, 3.5 mmol) in chloroform was added. After 7 hours, methanol (5 mL) and trimethylsilyl diazomethane (2.5 mL, 0.005 mole) was added to the reaction mixture. After 1 hour, glacial acetic acid (3 mL) was added with gas evolution observed. The solution was stirred for 0.5 hour. The product mixture was concentrated under vacuum. The residual material was subjected to column chromatography on silica gel eluting with 0-100% ethyl acetate in hexanes. The appropriate fractions were combined and concentrated to afford the title compound as a foam.

後処理

  1. waitAfter 7 hours
  2. waitAfter 1 hour
  3. stirringThe solution was stirred for 0.5 hour
  4. concentrationThe product mixture was concentrated under vacuum
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8ebc705357c0437f82017658c8347b56
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07598264B2

反応ノート

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