Water → 2-{[3-Methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethanol

HRID 85311노트

반응식

HRID 85311 반응식
[OH-].[Na+].O.[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH2:19][NH:20][CH2:21][CH2:22][O:23]C(=O)C(C)(C)C)[CH:9]=[CH:10][C:11]=1[CH:12]=[CH:13][C:14]1[S:15][CH:16]=[CH:17][CH:18]=1>C(O)C>[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH2:19][NH:20][CH2:21][CH2:22][OH:23])[CH:9]=[CH:10][C:11]=1[CH:12]=[CH:13][C:14]1[S:15][CH:16]=[CH:17][CH:18]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 68008944HCID 68008944, 화합물

생성물 1

HCID 680089612-{[3-Methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethanol

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
45 °C

실험 절차

NaOH (4.3 g, 107 mmol) was dissolved in ethanol (25 ml), and water (7 ml) was added thereto. Next, 2,2-dimethylpropionic acid 2-{[3-methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethyl ester (4.0 g, 10.7 mmol) was dissolved in ethanol (8 ml) and added dropwise to the mixture. The mixture was stirred at room temperature for 2 hours and further at 45° C. for 1 hour. After the solvent was evaporated off, water (100 ml) was added and the oily matter was subjected to extraction with ethyl acetate. After 2 times of washing with water, drying over Na2SO4 and concentration were performed. The residue was purified by silica gel chromatography to give a yellow oily matter (yield: 3.1 g (100%)).

후처리

  1. additionadded dropwise to the mixture
  2. customAfter the solvent was evaporated off
  3. additionwater (100 ml) was added
  4. extractionthe oily matter was subjected to extraction with ethyl acetate
  5. washAfter 2 times of washing with water
  6. dry with materialdrying over Na2SO4 and concentration
  7. customThe residue was purified by silica gel chromatography
  8. customto give a yellow oily matter (yield: 3.1 g (100%))

출처 및 근거

ORD 기록
ord-46f212c4d6a142638df8ed39582b9f84
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846955B2

반응 노트

불러오는 중…