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Sodium Hydroxide → 3-[2-Azido-2-(2-hydroxyethoxy)ethoxy]benzoic acid

HRID 661192
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반응식

HRID 661192 반응식
C([O:3][C:4](=[O:21])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH2:12][CH:13]([N:18]=[N+:19]=[N-:20])[O:14][CH2:15][CH2:16][OH:17])[CH:6]=1)C.[OH-].[Na+]>C(O)C>[N:18]([CH:13]([O:14][CH2:15][CH2:16][OH:17])[CH2:12][O:11][C:7]1[CH:6]=[C:5]([CH:10]=[CH:9][CH:8]=1)[C:4]([OH:21])=[O:3])=[N+:19]=[N-:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 597717683-[2-Azido-2-(2-hydroxyethoxy)ethoxy]benzoic acid ethyl ester

생성물 1

HCID 597717663-[2-Azido-2-(2-hydroxyethoxy)ethoxy]benzoic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-[2-Azido-2-(2-hydroxy-ethoxy)-ethoxy]-benzoic acid ethyl ester (1.34 g, 4.55 mmol) was stirred with 4 M aqueous sodium hydroxide (11.4 ml, 45.5 mmol) and ethanol (11.4 ml) at room temperature. After 3 hrs, all the solvents were removed under reduced pressure and the residue was dissolved in 50 ml water. The solution was acidified with 1 N HCl to pH 2 and then extracted with DCM (3×50 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The title compound was obtained as a colourless solid (1.2 g, 98.7%). ES-MS, m/z 265.85 (M−1).

후처리

  1. customall the solvents were removed under reduced pressure
  2. dissolutionthe residue was dissolved in 50 ml water
  3. extractionextracted with DCM (3×50 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f5abda65cfdf47a99edd7d4671c5a57f
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084590B2

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