Hydrochloric Acid → 2-(4-methyl-1H-indol-3-yl)ethan-1-amine

HRID 1111103

反応式

HRID 1111103 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:16]=1[C:9]([CH2:10][C@@H:11](C(O)=O)[NH2:12])=[CH:8][NH:7]2.O.C(OCC)(=O)C.Cl>C1(CC2C=CC=CC=2)C=CC=CC=1>[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:16]=1[C:9]([CH2:10][CH2:11][NH2:12])=[CH:8][NH:7]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8857Ethyl AcetateHCID 1508864-Methyl-L-tryptophan

生成物 1

HCID 1880072-(4-methyl-1H-indol-3-yl)ethan-1-amine

試薬・触媒・溶媒 1

HCID 7580Diphenylmethane溶媒

実験手順

A suspension of 4-methyltryptophan (1.14 g, 5.2 mmol, Sigma) in diphenylmethane (45 mL) was heated at reflux until complete solution was obtained. The solution was then mixed with 45 mL water and 45 mL ethyl acetate, and the pH brought to 1 or lower with concentrated HCl. The mixture was vortexed vigorously for 30 seconds, and centrifuged to provide three layers. The middle (aqueous) layer was washed with ethyl acetate, and adjusted to pH 10 or higher with 10 N NaOH. The resulting white precipitate was extracted into ethyl acetate, and the extract evaporated to dryness under vacuum, to yield crude 4-methyltryptamine base. The crude base was dissolved and acidified in 50 mL EtOH containing 6 mmol 6 N HCl, and the resulting 4-methyltryptamine hydrochloride was crystallized from solution.

後処理

  1. temperaturewas heated
  2. temperatureat reflux until complete solution
  3. customwas obtained
  4. customto provide three layers
  5. washThe middle (aqueous) layer was washed with ethyl acetate
  6. extractionThe resulting white precipitate was extracted into ethyl acetate
  7. customthe extract evaporated to dryness under vacuum

出典と根拠

ORDレコード
ord-c26a7c9929ea4f548d255b0b40fc386a
出典データセット
uspto-grants-1990_12
特許番号
US04978669

関連ノート

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