Sodium Bicarbonate → HCID 57594302, 화합물

HRID 730335노트

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HRID 730335 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C@H:12]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:13][CH2:14][OH:15])=[CH:7][CH:6]=1)=O.[NH2:24][C:25]1[C:30]([CH:31]([OH:33])[CH3:32])=[CH:29][CH:28]=[CH:27][N:26]=1.C(=O)(O)[O-].[Na+]>C(O)(C)C>[OH:15][CH2:14][CH2:13][C@@H:12]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2[N:24]=[C:25]3[C:30]([CH:31]([OH:33])[CH3:32])=[CH:29][CH:28]=[CH:27][N:26]3[CH:2]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 447548961-(2-Aminopyridin-3-yl)ethanolHCID 575947321,1-dimethylethyl ((1S)-1-{[4-(bromoacetyl)phenyl]methyl}-3-hydroxypropyl)carbamate

생성물 1

HCID 57594302HCID 57594302, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 1,1-dimethylethyl ((1S)-1-{[4-(bromoacetyl)phenyl]methyl}-3-hydroxypropyl)carbamate (1.00 g, 2.59 mmol), 1-(2-amino-3-pyridinyl)ethanol (0.358 g, 2.59 mmol), and solid sodium bicarbonate (0.272 g, 3.24 mmol) in isopropanol (25 mL) was heated at reflux for 3.5 h. and concentrated in vacuo. The residue was dissolved in ethyl acetate, washed with water and brine, dried (Na2SO4), and concentrated. The resulting pale yellow solid was used in the next reaction without further purification. MS(ES+) m/e 426 [M+H]+.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 3.5 h.
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water and brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated
  8. customThe resulting pale yellow solid was used in the next reaction without further purification

출처 및 근거

ORD 기록
ord-f0a63abdee7b4e7380d87c356dbc8412
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582668B2

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