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1-Butanol → HCID 131710330、化合物

HRID 1578283
ノート
印刷プレビュー

反応式

HRID 1578283 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 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 from a mixture solvent of methanol and ether

出典と根拠

ORDレコード
ord-9934f3f9a33d49e8a5458a1a4ae917be
出典データセット
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04292320

反応ノート

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