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1-Butanol → 1-(N-ethoxycarbonyl-p-chloroanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride

HRID 27149
ノート
印刷プレビュー

反応式

HRID 27149 の反応式
C(O[CH:4](OCC)[CH2:5][N:6]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)C.Cl.[OH:23][C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][C:32]=1[OH:33])[CH2:27][CH2:28][NH2:29].C(O)CCC.Cl>O>[ClH:13].[CH2:17]([O:16][C:14]([N:6]([CH2:5][CH:4]1[C:30]2[C:26](=[CH:25][C:24]([OH:23])=[C:32]([OH:33])[CH:31]=2)[CH2:27][CH2:28][NH:29]1)[C:7]1[CH:8]=[CH:9][C:10]([Cl:13])=[CH:11][CH:12]=1)=[O:15])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 2631-ButanolHCID 313Hydrochloric AcidHCID 65340Dopamine HydrochlorideHCID 20460556N-ethoxycarbonyl-p-chloroanilinoacetaldehyde diethyl acetal

生成物 1

HCID 204605721-(N-ethoxycarbonyl-p-chloroanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

N-ethoxycarbonyl-p-chloroanilinoacetaldehyde diethyl acetal (3.0 g) and 3,4-dihydroxyphenethylamine hydrochloride (1.5 g) were added to a mixture of n-butyl alcohol (30 ml), water (5 ml) and 10% hydrochloric acid (0.5 ml), and then the mixture was refluxed for 4 hours in a stream of nitrogen. Above mentioned acetal (0.8 g) was further added to the mixture and the resultant mixture was refluxed for 4 hours. The solvent was distilled off from the reaction mixture and the residue was washed with ethyl acetate and then recrystallized from water to give 1-(N-ethoxycarbonyl-p-chloroanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride, mp 208° to 210° C. and mp 214° to 215° C. Analysis: Calcd. for C19H21N2O4Cl.HCl.3/10H2O: C 54.50, H 5.44, N 6.69, Cl 16.93. Measured: C 54.29, H 5.57, N 6.70, Cl 16.69.

後処理

  1. temperaturethe mixture was refluxed for 4 hours in a stream of nitrogen
  2. additionwas further added to the mixture
  3. distillationThe solvent was distilled off from the reaction mixture
  4. washthe residue was washed with ethyl acetate
  5. customrecrystallized from water

出典と根拠

ORDレコード
ord-690f05e8f4c04db7ac3665b77d3a8ce2
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04220647

反応ノート

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