Water → Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-

HRID 1029997노트

반응식

HRID 1029997 반응식
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[CH:7][C:6]=1[N:13]1[CH2:17][CH2:16][O:15]C1=O.O>C(O)(=O)C>[CH3:11][C:9]1[CH:10]=[C:5]([O:4][CH3:3])[C:6]([NH:13][CH2:17][CH2:16][OH:15])=[CH:7][C:8]=1[OH:12]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 19821132HCID 19821132, 화합물

생성물 1

HCID 9794190Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-수율 45.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
70 °C

실험 절차

10 ml of 5N sodium hydroxide was heated to 70° C., and 2.76 g (12.4 mmol) of N-(2-methoxy-4-methyl-5-hydroxyphenyl)-1,3-oxazolidin-2-one was added thereto, and then the resulting mixture was stirred at 70° C. for 1 hour. After allowing to cool, 40 ml of water was poured into the reaction mixture, and acetic acid was added thereto until no further crystals were precipitated. The crystals were filtered, washed with water and recrystallized from the solvent mixture of water/ethanol (4:1, by volume). Thus, 1.10 g (5.6 mmol) of 2-methyl-4-methoxy-5-(β-hydroxyethylamino)phenol was obtained. The yield was 45%.

후처리

  1. temperatureto cool
  2. additionwas added
  3. customuntil no further crystals were precipitated
  4. filtrationThe crystals were filtered
  5. washwashed with water
  6. customrecrystallized from the solvent mixture of water/ethanol (4:1, by volume)

출처 및 근거

ORD 기록
ord-a04b393520c14199922277890d2a3cfc
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104414

반응 노트

불러오는 중…