Methylamine → 2,6-Dihydroxybenzamide

HRID 1375663

반응식

HRID 1375663 반응식
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:11])[C:3]=1[C:4]([O-])=[O:5].C[NH2:13].C1COCC1>>[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:11])[C:3]=1[C:4]([NH2:13])=[O:5]

참가 물질

4

반응물 3

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 178524827HCID 178524827, 화합물

생성물 1

HCID 766022,6-Dihydroxybenzamide

반응 조건

온도
100 °C

실험 절차

The mixture of 2,6-dihydroxybenzoate (168 mg, 1.0 mmol) and 2M methylamine in THF (3 mL, 6.0 mmol) in a sealed tube was heated at 100° C. overnight. The reaction mixture was then concentrated under reduced pressure and purified by flash chromatography on silica gel with hexane/ethyl acetate (1:1) to provide the titled compound (67 mg) as white solid. MS (ESI(+)) m/e 168 (M+H)+; 1H NMR (300 MHz, DMSO-d6) δ 12.57(bs, 2H), 8.82 (bs, 1H), 7.14 (t, J=8.1 Hz 1H), 6.35 (d, J=8.5 Hz, 2H), 2.85(d, J=4.7 Hz, 3H).

후처리

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. custompurified by flash chromatography on silica gel with hexane/ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-da5fe825a751428e93e4036d6b0144b8
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07169797B2

연결된 노트

불러오는 중…