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1-Butanol → HCID 131710330、化合物

HRID 1658327
ノート
印刷プレビュー

反応式

HRID 1658327 の反応式
C(O)CCC.[ClH:6].[OH:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:16]=1[OH:17])[CH2:11][CH2:12][NH2:13].C(O[CH:21](OCC)[CH2:22][S:23][C:24]1[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=1)C>Cl.O>[ClH:6].[CH3:30][C:27]1[CH:28]=[CH:29][C:24]([S:23][CH2:22][CH:21]2[C:14]3[C:10](=[CH:9][C:8]([OH:7])=[C:16]([OH:17])[CH:15]=3)[CH2:11][CH2:12][NH:13]2)=[CH:25][CH:26]=1
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 3

HCID 2631-ButanolHCID 65340Dopamine HydrochlorideHCID 7015317(2,2-Diethoxyethyl)(p-tolyl)sulfane

生成物 1

HCID 131710330HCID 131710330、化合物収率 106.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 962Water溶媒

実験手順

To a mixture of n-butanol (10 ml), water (2.5 ml) and concentrated hydrochloric acid (1 drop) were added 3,4-dihydroxyphenethylamine hydrochloride (0.63 g) and (4-methylthiophenoxy)acetaldehyde diethyl acetal (1.0 g), and the mixture was refluxed for 5 hours. After the reaction, the reaction mixture was concentrated to dryness under reduced pressure. The residue was crystallized by adding acetone, and the crystals were recrystallized by adding acetone, and the crystals were recryatallized from a mixture solvent of methanol and ether to give 1-(4-methylthiophenoxy)methyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride (1.2 g), mp 270°C (dec.).

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. customAfter the reaction
  3. concentrationthe reaction mixture was concentrated to dryness under reduced pressure
  4. customThe residue was crystallized
  5. additionby adding acetone
  6. customthe crystals were recrystallized
  7. additionby adding acetone

出典と根拠

ORDレコード
ord-7de35176a47c47d3b07429883a883ca5
出典データセット
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03963725

反応ノート

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