Butylamine → Trans-4-n-butylamino-1-ethyl-3-pyrrolidinol

HRID 126928노트

반응식

HRID 126928 반응식
[O:1]1[CH:6]2[CH:2]1[CH2:3][N:4]([CH2:7][CH3:8])[CH2:5]2.[CH2:9]([NH2:13])[CH2:10][CH2:11][CH3:12]>Cl>[CH2:9]([NH:13][C@@H:2]1[CH2:3][N:4]([CH2:7][CH3:8])[CH2:5][C@H:6]1[OH:1])[CH2:10][CH2:11][CH3:12]

참가 물질

4

반응물 2

HCID 8007ButylamineHCID 13320194N-ethyl-3,4-epoxypyrrolidine

생성물 1

HCID 70563799Trans-4-n-butylamino-1-ethyl-3-pyrrolidinol

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

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온도
150 °C

실험 절차

A mixture of 22.6 g (0.20 mole) of 3,4-epoxy-1-ethyl-pyrrolidine, 29.2 g (0.40 mol) of n-butylamine and one drop of conc. hydrochloric acid was heated in a bomb at 150° C. for 20 hr. The mixture was cooled to room temperature, diluted with 350 ml of petroleum ether, cooled in an ice bath and the precipitate was collected. The yield of pure compound as white flakes in this step was 18.0 g (48%); m.p. 57.5°-59.0° C. The filtrate was concentrated under high vaccum leaving a residue of 17.5 g (47%) of quite pure product. Total yield in the two steps was 35.5 g (about 95%).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. temperaturecooled in an ice bath
  3. customthe precipitate was collected
  4. concentrationThe filtrate was concentrated under high vaccum
  5. customleaving a residue of 17.5 g (47%) of quite pure product
  6. customTotal yield in the two steps

출처 및 근거

ORD 기록
ord-fcd5792b438d476594c4442b5cab0aba
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254135

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