Hydrochloric Acid → HCID 21403372、化合物

HRID 973043ノート

反応式

HRID 973043 の反応式
C([O:8][C:9]1[CH:18]=[C:17]([O:19]CC2C=CC=CC=2)[CH:16]=[C:15]2[C:10]=1[CH:11]=[CH:12][N:13]=[C:14]2[CH2:27][C:28]1[CH:33]=[C:32]([O:34][CH3:35])[C:31]([O:36][CH3:37])=[C:30]([O:38][CH3:39])[CH:29]=1)C1C=CC=CC=1.[ClH:40].C(O)C.Cl.C(O)C>[H][H].[Pt](=O)=O>[ClH:40].[OH:8][C:9]1[CH:18]=[C:17]([OH:19])[CH:16]=[C:15]2[C:10]=1[CH2:11][CH2:12][NH:13][CH:14]2[CH2:27][C:28]1[CH:33]=[C:32]([O:34][CH3:35])[C:31]([O:36][CH3:37])=[C:30]([O:38][CH3:39])[CH:29]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 12707063HCID 12707063、化合物HCID 21887872Ethanol hydrochloride

生成物 1

HCID 21403372HCID 21403372、化合物

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

A mixture of 1.4 g of 5,7-dibenzyloxy-1-(3,4,5-trimethoxybenzyl)-isoquinoline, 0.7 g of platinum dioxide, 100 ml of a hydrochloric acid-ethanol solution (the content of hydrochloric acid: 9%) and 50 ml of ethanol is shaken at 25° C in hydrogen atmosphere. After 150 ml of hydrogen are absorbed, the catalyst is removed by filtration. The filtrate is evaporated to remove solvent, whereby a mixture of 5,7-dihydroxy-1-(3,4,5-trimethoxybenzyl)-isoquinoline hydrochloride and 5,7-dihydroxy-1-(3,4,5-trimethoxybenzyl)-1,2,3,4-tetrahydroisoquinoline hydrochloride is obtained. This mixture is recrystallized 33 times from ethanol, whereby 0.3 g of 5,7-dihydroxy-1-(3,4,5-trimethoxybenzyl)-1,2,3,4-tetrahydrolsoquinoline hydrochloride is obtained. Yield: 40% The physiocochemical properties of this product are identical with those of the compound obtained in Example 1.

後処理

  1. customAfter 150 ml of hydrogen are absorbed
  2. customthe catalyst is removed by filtration
  3. customThe filtrate is evaporated
  4. customto remove solvent, whereby
  5. additiona mixture of 5,7-dihydroxy-1-(3,4,5-trimethoxybenzyl)-isoquinoline hydrochloride

出典と根拠

ORDレコード
ord-15114816061a4ba4858e5eac3ab30735
出典データセット
uspto-grants-1977_10
特許番号
US04054659

反応ノート

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