Nitrate → 4-Nitroxymethylpiperidine nitrate

HRID 1086486

반응식

HRID 1086486 반응식
[OH:1][CH2:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.[N+:9]([O-:12])([OH:11])=[O:10].[N+:13]([O-])([O:15]C(=O)C)=[O:14].C(OC(C)C)(C)C.[N+]([O-])([O-])=O>C(#N)C>[N+:9]([O-:12])([OH:11])=[O:10].[O:1]([CH2:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)[N+:13]([O-:15])=[O:14]

참가 물질

7

반응물 5

HCID 943NitrateHCID 944Nitric Acid2회HCID 7914Diisopropyl EtherHCID 11557Acetyl nitrateHCID 4207714-Piperidinemethanol

생성물 1

HCID 532305974-Nitroxymethylpiperidine nitrate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

5.8 g. 4-Hydroxymethylpiperidine are dissolved in 100 ml. acetonitrile and cooled to -25° C. By the addition of 3.1 ml. 100% nitric acid, the base is converted into the nitric acid salt. To this solution is added a freshly prepared acetyl nitrate solution (prepared from 9.5 ml. acetic anhydride and 4.2 ml. 100% nitric acid in 40 ml. acetonitrile at -25° C.) and the reaction mixture then stirred for 3 hours at this temperature. The reaction solution is diluted with 300 ml. diisopropyl ether. The crystals obtained are filtered off with suction and washed with diethyl ether. There are obtained 9.5 g. (82% of theory) of the nitrate of the title compound; m.p. 64°-65° C.

후처리

  1. additionBy the addition of 3.1 ml
  2. additionThe reaction solution is diluted with 300 ml
  3. customThe crystals obtained
  4. filtrationare filtered off with suction
  5. washwashed with diethyl ether
  6. customThere are obtained 9.5 g

출처 및 근거

ORD 기록
ord-0171ce45626b4b4bae07029045f81c13
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05030641

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