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Dopamine Hydrochloride → HCID 70505289、化合物

HRID 543730
ノート
印刷プレビュー

反応式

HRID 543730 の反応式
Cl.[OH:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[OH:12])[CH2:6][CH2:7][NH2:8].C([O:15][CH:16]([O:29]CC)[CH2:17][NH:18][C:19]([O:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:20])C>C(O)CCC.O>[C:16]([OH:29])(=[O:15])[CH3:17].[CH2:22]([O:21][C:19]([NH:18][CH2:17][CH:16]1[C:9]2[C:5](=[CH:4][C:3]([OH:2])=[C:11]([OH:12])[CH:10]=2)[CH2:6][CH2:7][NH:8]1)=[O:20])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 65340Dopamine HydrochlorideHCID 292521Benzyl 2,2-diethoxyethylcarbamate

生成物 1

HCID 70505289HCID 70505289、化合物収率 41.3%

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 962Water溶媒

実験手順

A solution of 3,4-dihydroxyphenethylamine hydrochloride (2.17 g) and N-benzyloxycarbonylaminoacetaldehyde diethyl acetal (4.0 g) in a mixture of n-butyl alcohol (20 ml) and water (3.5 ml) was refluxed for 4.5 hours. After the reaction, the solvent was distilled off under reduced pressure. To the residue were added water (15 ml) and sodium acetate. A precipitating oil was separated from the aqueous layer and chloroform was added thereto. The mixture was allowed to stand to give crystals. The crystals were collected by filtration, washed with chloroform and recrystallized twice from a mixture of methanol and ether to give 1(N-benzyloxycarbonylaminomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline acetate (1.2 g), mp 158° to 162° C. (dec).

後処理

  1. temperaturewas refluxed for 4.5 hours
  2. customAfter the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionTo the residue were added water (15 ml) and sodium acetate
  5. customA precipitating oil was separated from the aqueous layer and chloroform
  6. additionwas added
  7. customto give crystals
  8. filtrationThe crystals were collected by filtration
  9. washwashed with chloroform
  10. customrecrystallized twice from a mixture of methanol and ether

出典と根拠

ORDレコード
ord-72dd53aaed28448c9852ab00b2016ce1
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04447436

反応ノート

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