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

HRID 126928ノート

反応式

HRID 126928 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid触媒

反応条件

温度
150 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-fcd5792b438d476594c4442b5cab0aba
出典データセット
uspto-grants-1981_03
特許番号
US04254135

反応ノート

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