Methanol → 1-Aminocarbonyl-4-nitroxypiperidine

HRID 1198140노트

반응식

HRID 1198140 반응식
[O:1]([CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)[N+:2]([O-:4])=[O:3].O.CO.[O-:14][C:15]#[N:16].[K+]>C(O)(=O)C>[NH2:16][C:15]([N:8]1[CH2:9][CH2:10][CH:5]([O:1][N+:2]([O-:4])=[O:3])[CH2:6][CH2:7]1)=[O:14]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 11378442Potassium cyanateHCID 15068866HCID 15068866, 화합물

생성물 1

HCID 150688551-Aminocarbonyl-4-nitroxypiperidine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

7.1 g. 4-Nitroxypiperidine are dissolved in 60 ml. water and 30 ml. methanol and mixed with 16.2 g. potassium cyanate. After the dropwise addition of 12 ml. glacial acetic acid, stirring is continued at ambient temperature for 4 hours. The inorganic salts are precipitated out by the addition of 100 ml. ethyl acetate. After suction filtration, the aqueous phase is separated off and the organic phase is dried with anhydrous sodium sulphate. After suction filtration, the filtrate is evaporated in a vacuum. The residue is triturated with diethyl ether and the crystals are filtered off with suction. There are obtained 8.3 g. of the title compound, i.e. 89% of theory; m.p. 110°-111° C.

후처리

  1. additionAfter the dropwise addition of 12 ml
  2. customThe inorganic salts are precipitated out by the addition of 100 ml
  3. filtrationAfter suction filtration
  4. customthe aqueous phase is separated off
  5. dry with materialthe organic phase is dried with anhydrous sodium sulphate
  6. filtrationAfter suction filtration
  7. customthe filtrate is evaporated in a vacuum
  8. customThe residue is triturated with diethyl ether
  9. filtrationthe crystals are filtered off with suction
  10. customThere are obtained 8.3 g

출처 및 근거

ORD 기록
ord-3f33edc990c240d8a7c498c6651f32ff
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05280031

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