Lithium Hydroxide → HCID 24959696、化合物

HRID 2381853ノート

反応式

HRID 2381853 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([N:7]2[N:11]=[N:10][C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[N:8]2)[S:4][C:3]=1[C:18]([O:20]CC)=[O:19].O1CCCC1.[OH-].[Li+]>O>[CH3:1][C:2]1[CH:6]=[C:5]([N:7]2[N:11]=[N:10][C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[N:8]2)[S:4][C:3]=1[C:18]([OH:20])=[O:19]

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 24959335HCID 24959335、化合物

生成物 1

HCID 24959696HCID 24959696、化合物収率 82.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of ethyl 3-methyl-5-(5-phenyl-2H-tetrazol-2-yl)thiophene-2-carboxylate (0.16 g, 0.51 mmol) in a 1:1 mixture of tetrahydrofuran:water (10 mL) was added lithium hydroxide (0.11 g, 2.55 mmol). The reaction mixture was refluxed for 18 hours and allowed to cool to ambient temperature. The organic solvent was removed in vacuo. The aqueous solution was acidified with 10% aqueous solution. The white solid was collected by filtration, washed with water and dried to afford the title compound as red colored solid (0.12 g, 82%): 1H NMR (300 MHz, DMSO-d6) δ 8.14-8.11 (m, 2H), 7.75 (s, 1H), 7.62-7.60 (m, 3H), 2.54 (s, 3H); MS (ES+) m/z 287.2 (M+1).

後処理

  1. temperatureThe reaction mixture was refluxed for 18 hours
  2. customThe organic solvent was removed in vacuo
  3. filtrationThe white solid was collected by filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-b687c5d01b56436ea56ff8b1219cb8a3
出典データセット
uspto-grants-2012_09
特許番号
US08258160B2

反応ノート

読み込み中…