Isopropylamine → 1-[(3-Chloropyrazin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

HRID 1701739ノート

反応式

HRID 1701739 の反応式
Br[CH2:2][CH:3]([OH:13])[CH2:4][O:5][C:6]1[C:11]([Cl:12])=[N:10][CH:9]=[CH:8][N:7]=1.[CH:14]([NH2:17])([CH3:16])[CH3:15]>CO>[Cl:12][C:11]1[C:6]([O:5][CH2:4][CH:3]([OH:13])[CH2:2][NH:17][CH:14]([CH3:16])[CH3:15])=[N:7][CH:8]=[CH:9][N:10]=1

参加物

4

反応物 2

HCID 6363IsopropylamineHCID 204834011-Bromo-3-[(3-chloropyrazin-2-yl)oxy]propan-2-ol

生成物 1

HCID 204834181-[(3-Chloropyrazin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

53 g of 2-(3'-bromo-2'-hydroxy-propoxy)-3-chloropyrazine and 59 g of isopropylamine in 500 ml of methanol are boiled for 15 hours under reflux. The reaction mixture is then evaporated in a waterpump vacuum. The residue is partitioned between 2 N hydrochloric acid and ether. The hydrochloric acid phase is rendered alkaline with concentrated sodium hydroxide solution and extracted by shaking with ether. The ether extracts are washed with water, dried over sodium sulphate and evaporated in a waterpump vacuum. The residue crystallises from ether. 3-Chloro-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine, melting point 99°-100° C., is thus obtained.

後処理

  1. temperatureunder reflux
  2. customThe reaction mixture is then evaporated in a waterpump vacuum
  3. customThe residue is partitioned between 2 N hydrochloric acid and ether
  4. extractionextracted
  5. washThe ether extracts are washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated in a waterpump vacuum
  8. customThe residue crystallises from ether

出典と根拠

ORDレコード
ord-dd3b342910b94f97813d6cc854fea4c2
出典データセット
uspto-grants-1980_03
特許番号
US04195090

反応ノート

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