Sodium Methoxide → HCID 20483476、化合物

HRID 1701741ノート

反応式

HRID 1701741 の反応式
[Cl:1][C:2]1[C:3]([O:8][CH2:9][CH:10]([OH:16])[CH2:11][NH:12][CH:13]([CH3:15])[CH3:14])=[N:4][CH:5]=[CH:6][N:7]=1.[CH3:17][O-:18].[Na+]>CO>[ClH:1].[CH3:17][O:18][C:2]1[C:3]([O:8][CH2:9][CH:10]([OH:16])[CH2:11][NH:12][CH:13]([CH3:15])[CH3:14])=[N:4][CH:5]=[CH:6][N:7]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 204834181-[(3-Chloropyrazin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

生成物 1

HCID 20483476HCID 20483476、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

7.5 g of 3-chloro-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine and 3.2 g of sodium methylate in 150 ml of methanol are boiled for 10 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 acid aqueous 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 crude base is thus obtained, from which 3-methoxy-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine hydrochloride, melting point 152°-153° C., is obtained by reaction with ethereal hydrochloric acid in methanol.

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

出典と根拠

ORDレコード
ord-ee198cdb44454aa3a32b3279f8c0b005
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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