Nitric Acid → 3-Nitroxypropylamine nitrate

HRID 8085

반응식

HRID 8085 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].[N+:6]([O-:9])([OH:8])=[O:7]>C(OC(=O)C)(=O)C>[N+:6]([O-:9])([OH:8])=[O:7].[N+:6]([O:5][CH2:4][CH2:3][CH2:2][NH2:1])([O-:8])=[O:7]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 90863-Amino-1-propanol

생성물 1

HCID 220145913-Nitroxypropylamine nitrate수율 80%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

A solution of 3-amino-1-propanol (6.17 g, 82.2 mmol) was added, dropwise, to an ice-cooled solution of fuming nitric acid (12 mL) in acetic anhydride (50 mL). The reaction was stirred in an ice-bath for 10 minutes and then at room temperature for 10 minutes. The solvent was evaporated under vacuum at 40° C. The residue was stirred in diethyl ether (200 mL) until the product precipitated. The mixture was filtered and the white crystalline solid was dried in vacuo to give the title compound (12.1 g, 80% yield). 1H NMR (DMSO-d6) δ 4.57 (br. t, 2 H), 2.8–3.0 (m, 2H), 1.96 (m, 2H). 13C NMR (DMSO-d6) δ 70.9, 36.1, 24.5. MS(API) m/z 121 (M−NO3)+.

후처리

  1. waitat room temperature for 10 minutes
  2. customThe solvent was evaporated under vacuum at 40° C
  3. stirringThe residue was stirred in diethyl ether (200 mL) until the product
  4. customprecipitated
  5. filtrationThe mixture was filtered
  6. customthe white crystalline solid was dried in vacuo

출처 및 근거

ORD 기록
ord-fd95e3c9024b41f58c60e5039c57717d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087630B2

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