Sodium Azide → HCID 23044225, 화합물

HRID 1762581노트

반응식

HRID 1762581 반응식
[N-:1]=[N+:2]=[N-:3].[Na+].[CH3:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][CH2:12][CH:13]([CH2:17]OS(C3C=CC(C)=CC=3)(=O)=O)[CH2:14]2)=[CH:9][CH:8]=1>O.C(O)C>[CH3:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][CH2:12][CH:13]([CH2:17][N:1]=[N+:2]=[N-:3])[CH2:14]2)=[CH:9][CH:8]=1

참가 물질

5

반응물 2

HCID 33557Sodium AzideHCID 11210176p-Toluenesulphonic acid (7-methoxy-1,2,3,4-tetrahydro-naphth-2-ylmethyl) ester

생성물 1

HCID 23044225HCID 23044225, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 3.9 g of sodium azide in 10 ml of water is added to a solution of 13.86 g (40 mmol) of p-toluenesulphonic acid (7-methoxy-1,2,3,4-tetrahydro-naphth-2-ylmethyl) ester in 200 ml of ethanol and the whole is boiled under reflux for 18 hours. After cooling, the alcohol is evaporated off under reduced pressure, water is added to the residue and extraction is carried out with dichloromethane. The organic phase is washed with water, dried over sodium sulphate and concentrated by evaporation. (7-methoxy-1,2,3,4-tetrahydro-naphth-2-yl)methylazide is obtained in the form of a yellow oil.

후처리

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling
  3. customthe alcohol is evaporated off under reduced pressure, water
  4. additionis added to the residue and extraction
  5. washThe organic phase is washed with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-f745d8a6cc764a8cb47e48a23f9119e2
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833169

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