Hydrochloric Acid → 3-Isoquinolinecarboxylic acid,1,2,3,4-tetrahydro-6-hydroxy-,hydrochloride

HRID 1199669ノート

反応式

HRID 1199669 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][CH:13]=1)[CH2:5][C@@H:6]([C:8]([OH:10])=[O:9])[NH2:7].[CH2:14]=O.[ClH:16]>>[ClH:16].[OH:1][C:2]1[CH:3]=[C:4]2[C:11](=[CH:12][CH:13]=1)[CH2:14][NH:7][CH:6]([C:8]([OH:10])=[O:9])[CH2:5]2

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 6950578L-m-tyrosine

生成物 1

HCID 129261753-Isoquinolinecarboxylic acid,1,2,3,4-tetrahydro-6-hydroxy-,hydrochloride

実験手順

To a mixture of 100.0 g of 3-hydroxyphenylalanine in 820 ml of 5% hydrochloric acid were added 78 ml of formaldehyde (37% in water). The reaction mixture was heated at 90°-95° C. (external bath temperature) for 45 minutes. The mixture was cooled and concentrated in vacuo. Five hundred milliliters of ethanol were added and the mixture was again concentrated in vacuo, affording 115 g of the title intermediate as a pale white solid, used without purification in the next step.

後処理

  1. temperatureThe reaction mixture was heated at 90°-95° C. (external bath temperature) for 45 minutes
  2. temperatureThe mixture was cooled
  3. concentrationconcentrated in vacuo
  4. additionFive hundred milliliters of ethanol were added
  5. concentrationthe mixture was again concentrated in vacuo

出典と根拠

ORDレコード
ord-3e46a5c4658f44709ace3d572789c3f3
出典データセット
uspto-grants-1990_02
特許番号
US04902695

反応ノート

読み込み中…