Water → HCID 18173786, 화합물

HRID 2399880노트

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HRID 2399880 반응식
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1.[N-:14]=[N+:15]=[N-:16].[Li+].O>CN(C=O)C>[N:14]([CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[N+:15]=[N-:16]

참가 물질

5

반응물 3

HCID 962WaterHCID 88163Lithium azideHCID 27645871-(2-Chloroethoxy)-4-nitrobenzene

생성물 1

HCID 18173786HCID 18173786, 화합물수율 97%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 1.12 g (5.55 mmol) of 4-nitro 2-chloroethyl ether (Example 212) and lithium azide (544 mg, 11.1 mmol) in 3 mL of DMF was heated at 60° C. in an oil bath overnight under nitrogen atmosphere. The reaction was poured into water and extracted with ethyl acetate. The organics were washed with water and brine and dried over anhydrous magnesium sulfate and concentrated to give 1.12 g (97%) of the product: 1H NMR (200 MHz, CDCl3) δ8.18 (d, 2H, J=9Hz), 6.96 (d, 2H, J=9Hz), 4.21 (t, 2H, J=5Hz), 3.63 (t, 2H, J=5Hz).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organics were washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e21c0ad2a5874e68ba920e261cbc5836
출처 데이터셋
uspto-grants-1995_09
특허 번호
US05451677

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