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Dopamine Hydrochloride → HCID 70505289, 화합물

HRID 543730
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HRID 543730 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 65340Dopamine HydrochlorideHCID 292521Benzyl 2,2-diethoxyethylcarbamate

생성물 1

HCID 70505289HCID 70505289, 화합물수율 41.3%

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-72dd53aaed28448c9852ab00b2016ce1
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04447436

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