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Sodium Azide → HCID 20245092, 화합물

HRID 1075397
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HRID 1075397 반응식
[O:1]([CH2:8][CH2:9][C:10](Cl)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N-:13]=[N+:14]=[N-:15].[Na+]>CC(C)=O.O>[O:1]([CH2:8][CH2:9][C:10]([N:13]=[N+:14]=[N-:15])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 33557Sodium AzideHCID 1199233-Phenoxypropionyl chloride

생성물 1

HCID 20245092HCID 20245092, 화합물수율 68.2%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

Phenoxypropionyl chloride (9.23 g, 0.05 mol) is dissolved in 100 ml acetone and cooled with an ice bath as sodium azide (3.6 g, 0.055 mol) in 10 ml water is added dropwise. After addition is completed, the reaction mixture is warmed to room temperature and stirred for 30 minutes. The solution is decanted and concentrated. The residue is dissolved in 100 ml ether and washed with saturated sodium bicarbonate and brine. The organic phase is separated, dried (MgSO4) and concentrated to give 6.52 g (68.0% yield) of phenoxypropionyl azide as a yellow oil which solidifies on cooling. IR (KBr) cm-1 : 2137 (N3), 1718 (C=O); 1H nmr (CDCl3) δ: 7.31 (m, 2H, phenyl H), 6.98 (t, 1H, J=7.5 Hz, phenyl H), 6.92 (m, 2H, phenyl H), 4.26 (t, 3H, J=6.3 Hz, CH2O), 2.84 (t, 3H, J=6.3 Hz, CH2C=O); 13C nmr (CDCl3) δ: 178.0, 159.0, 129.5(2C), 121.2, 114.7(2C), 62.9, 36.9.

후처리

  1. additionis added dropwise
  2. additionAfter addition
  3. customThe solution is decanted
  4. concentrationconcentrated
  5. dissolutionThe residue is dissolved in 100 ml ether
  6. washwashed with saturated sodium bicarbonate and brine
  7. customThe organic phase is separated
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3afe03b625184ce28a002e0dde3435ba
출처 데이터셋
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05900485

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