Tryptamine hydrochloride → Kumujian A

HRID 628666

反応式

HRID 628666 の反応式
Cl.[NH2:2][CH2:3][CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1.[CH2:14]([O:16][C:17](=[O:20])[CH:18]=O)[CH3:15]>C(O)C.C1(C)C=CC=CC=1>[CH2:14]([O:16][C:17]([C:18]1[C:6]2[NH:7][C:8]3[C:13]([C:5]=2[CH:4]=[CH:3][N:2]=1)=[CH:12][CH:11]=[CH:10][CH:9]=3)=[O:20])[CH3:15]

参加物

5

反応物 2

HCID 67652Tryptamine hydrochlorideHCID 70211Ethyl oxoacetate

生成物 1

HCID 11701473Kumujian A

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1140Toluene溶媒

実験手順

To a suspension of tryptamine hydrochloride (2.00 g, 10.17 mmol) in ethanol (25 mL) was added a solution of glyoxylic acid ethyl ester (3.12 g, 15.26 mmol) in toluene (50% v/v) at 0° C. After the reaction mixture was stirred overnight at ambient temperature, the solvent was removed under reduced pressure. The resulting residue was treated with saturated aqueous sodium bicarbonate. The product was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. The crude product was used in the next step without further purification.

後処理

  1. customthe solvent was removed under reduced pressure
  2. additionThe resulting residue was treated with saturated aqueous sodium bicarbonate
  3. extractionThe product was extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was used in the next step without further purification

出典と根拠

ORDレコード
ord-3b814fa746c84ca6bacc617ccb47992d
出典データセット
uspto-grants-2016_04
特許番号
US09314468B2

関連ノート

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