Formic Acid → HCID 178523823, 화합물

HRID 35966

반응식

HRID 35966 반응식
[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]

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 8857Ethyl AcetateHCID 178511725HCID 178511725, 화합물

생성물 1

HCID 178523823HCID 178523823, 화합물수율 66.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e1b24c9a3ef84fc4ae523d33295482bf
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05411989

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