Hydrochloric Acid → HCID 59187024、化合物

HRID 1887248ノート

反応式

HRID 1887248 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=1.[OH-:16].[Na+].Cl>CO>[O:9]([CH2:8][C:6]1[CH:5]=[CH:4][NH:3][C:2](=[O:16])[CH:7]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 62472276HCID 62472276、化合物

生成物 1

HCID 59187024HCID 59187024、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
170 °C

実験手順

To a solution of 2-chloro-4-(phenoxymethyl)pyridine (2.34 g, 10.68 mmol) in anhydrous methanol (30 mL) in a steel bomb was added sodium hydroxide (3.20 g, 80.11 mmol). The reaction mixture was stirred at 170° C. for 16 hours, cooled to 0° C. and neutralized with cold concentrated hydrochloric acid, followed by the addition of methanol (10 mL) and filtration. The filtrate was concentrated in vacuo and the residue was washed with methanol and hexane. The title compound was obtained as a colorless solid in 93% (2 g): 1H NMR (300 MHz, CDCl3) δ 13.00 (br s, 1H), 7.35-7.25 (m, 3H), 6.99-6.90 (m, 3H), 6.64 (s, 1H), 6.34 (d, J=6.6 Hz, 1H), 4.93 (s, 2H); MS (ES+) m/z 202.2 (M+1).

後処理

  1. concentrationThe filtrate was concentrated in vacuo
  2. washthe residue was washed with methanol and hexane

出典と根拠

ORDレコード
ord-7c6cfa924afb4499bfac3dde2719e381
出典データセット
uspto-grants-2013_08
特許番号
US08501746B2

反応ノート

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