Nitrate → 4-Nitroxymethylpiperidine nitrate

HRID 1086486

反応式

HRID 1086486 の反応式
[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]

参加物

7

反応物 5

HCID 943NitrateHCID 944Nitric Acid2 回HCID 7914Diisopropyl EtherHCID 11557Acetyl nitrateHCID 4207714-Piperidinemethanol

生成物 1

HCID 532305974-Nitroxymethylpiperidine nitrate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0171ce45626b4b4bae07029045f81c13
出典データセット
uspto-grants-1991_07
特許番号
US05030641

関連ノート

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