Hydrochloric Acid → HCID 59187024, 화합물

HRID 1887248노트

반응식

HRID 1887248 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 62472276HCID 62472276, 화합물

생성물 1

HCID 59187024HCID 59187024, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
170 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-7c6cfa924afb4499bfac3dde2719e381
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501746B2

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