Lithium Hydroxide → HCID 18453190、化合物

HRID 45314

反応式

HRID 45314 の反応式
[O:1]=[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]1[C:8]1[CH:18]=[CH:17][C:11]([C:12]([O:14]CC)=[O:13])=[CH:10][CH:9]=1.[OH-].[Li+]>O1CCCC1.O>[O:1]=[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]1[C:8]1[CH:18]=[CH:17][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 16656197Ethyl 4-(2-oxopyridin-1(2H)-yl)benzoate

生成物 1

HCID 18453190HCID 18453190、化合物収率 85%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

反応条件

温度
70 °C

実験手順

A mixture of ethyl 4-(2-oxopyridin-1(2H)-yl)benzoate (0.40 g, 1.64 mmol) and lithium hydroxide (0.28 g, 6.60 mmol) in tetrahydrofuran/water mixture was stirred at 70° C. for 1 h. The organic solvent was removed in vacuo. The water layer was washed with ethyl acetate (25 mL) and then acidified by addition of 15% hydrochloric acid solution. The solid obtained was collected by filtration, washed with water and dried in air to afford the title compound in 85% yield (0.30 g); 1H NMR (300 MHz, DMSO-d6) δ 13.14 (s, 1H), 8.02 (d, J=8.4 Hz, 2H), 7.65 (dd, J=1.9, 6.9 Hz, 1H), 7.51 (d, J=8.5 Hz, 2H), 7.48 (dd, J=1.9, 6.9 Hz, 1H), 6.47 (d, J=9.2 Hz, 1H), 6.31 (dt, J=1.0, 6.9 Hz, 1H).

後処理

  1. customThe organic solvent was removed in vacuo
  2. washThe water layer was washed with ethyl acetate (25 mL)
  3. additionacidified by addition of 15% hydrochloric acid solution
  4. customThe solid obtained
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried in air

出典と根拠

ORDレコード
ord-f97c14b776d44f2381eee4f0fc9630da
出典データセット
uspto-grants-2013_09
特許番号
US08541457B2

関連ノート

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