홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium Hydroxide → 2,2-Dinitropropyl methyl ether

HRID 1981959
노트
인쇄 미리보기

반응식

HRID 1981959 반응식
[OH-].[Na+].[CH3:3][O:4][CH2:5][CH:6]([N+:8]([O-:10])=[O:9])[CH3:7].[N:11]([O-:13])=[O:12].[Na+].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>O.[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+].C(Cl)Cl>[CH3:3][O:4][CH2:5][C:6]([N+:11]([O-:13])=[O:12])([N+:8]([O-:10])=[O:9])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 136092852-Nitropropyl methyl etherHCID 23668193Sodium Nitrite

생성물 1

HCID 143235302,2-Dinitropropyl methyl ether수율 88.1%

시약·촉매·용매 3

HCID 178511488HCID 178511488, 화합물
촉매
HCID 962Water용매3회
HCID 6344Dichloromethane용매

실험 절차

A solution of 1.0 g (25 mmoles) of sodium hydroxide in 10 mL of water was treated with 2.0 g (16.8 mmoles) of 2-nitropropyl methyl ether. After 10 minutes, 10 mL of methylene chloride was added, followed by a solution of 5.0 g (72 mmoles) of sodium nitrite in 10 mL of water. Next, a solution of 1.0 g (3 mmoles) of potassium ferricyanide in 5 mL of water was added, followed by 4.4 g (18 mmoles) of solid sodium persulfate. A cold water bath was used to moderate exothermic reaction. After 30 minutes, the reaction mixture was extracted with two 15 mL portions of methylene chloride. The combined extracts were washed with brine and dried over anhydrous magnesium sulfate. The solution was distilled in a short-path distillation apparatus to give 2.43 g (88% yield) of 2,2-dinitropropyl methyl ether, a colorless liquid, b.p. 100° (16 mm). 'H NMR (CDCl3): &2.18 (s. 3 H, --CH3), 3.35 (s, 3 H, --OCH3), 4.15 (s, 2H, --CH2O).

후처리

  1. customA cold water bath was used
  2. customreaction
  3. waitAfter 30 minutes
  4. extractionthe reaction mixture was extracted with two 15 mL portions of methylene chloride
  5. washThe combined extracts were washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solution was distilled in a short-path distillation apparatus

출처 및 근거

ORD 기록
ord-61c8f481ec7d4aa2bdc1c9868b3d40a4
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04594430

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트