Formic Acid → HCID 178523823、化合物

HRID 35966

反応式

HRID 35966 の反応式
[C:1](OC(=O)C)(=[O:3])C.C(O)=O.[O:11]([C@H:15]1[CH2:20][CH2:19][C@H:18]([NH2:21])[CH2:17][CH2:16]1)[N+:12]([O-:14])=[O:13].C(OCC)(=O)C>O>[CH:1]([NH:21][C@H:18]1[CH2:17][CH2:16][C@H:15]([O:11][N+:12]([O-:14])=[O:13])[CH2:20][CH2:19]1)=[O:3]

参加物

6

反応物 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 8857Ethyl AcetateHCID 178511725HCID 178511725、化合物

生成物 1

HCID 178523823HCID 178523823、化合物収率 66.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 6.8 ml (0.072 mol) acetic acid anhydride and 2.8 ml (0.072 mol) formic acid is heated for 2 h to 60° C. and thereafter mixed, with cooling at 5° C., with 1.9 g (0.012 mol) trans-4-nitroxycyclohexylamine. One leaves to stir overnight at room temperature, subsequently dilutes with 100 ml ethyl acetate and adds 100 ml of water thereto. After neutralisation with saturated sodium hydrogen carbonate solution, the organic phase is dried with sodium sulphate and distilled off in a vacuum. After trituration with ether, the crystals are filtered off with suction. One obtains 1.5 g of the title compound of the m p 148°-150° C., i.e. 66% of theory.

後処理

  1. temperatureis heated for 2 h to 60° C.
  2. additionmixed
  3. customOne leaves
  4. dry with materialAfter neutralisation with saturated sodium hydrogen carbonate solution, the organic phase is dried with sodium sulphate
  5. distillationdistilled off in a vacuum
  6. filtrationAfter trituration with ether, the crystals are filtered off with suction

出典と根拠

ORDレコード
ord-e1b24c9a3ef84fc4ae523d33295482bf
出典データセット
uspto-grants-1995_05
特許番号
US05411989

関連ノート

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