Chloroacetonitrile → HCID 19837048、化合物

HRID 476876ノート

反応式

HRID 476876 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:11](=[CH:12][CH:13]=1)[C:7]([CH2:8][CH2:9][NH2:10])=[CH:6][NH:5]2.Cl[CH2:15][C:16]#[N:17]>O1CCCC1.C(Cl)Cl>[CH3:1][C:2]1[CH:3]=[C:4]2[C:11]([C:7]([CH2:8][CH2:9][NH:10][CH2:15][C:16]#[N:17])=[CH:6][NH:5]2)=[CH:12][CH:13]=1

参加物

5

反応物 2

HCID 7856ChloroacetonitrileHCID 1900062-(6-Methyl-1H-indol-3-yl)ethan-1-amine

生成物 1

HCID 19837048HCID 19837048、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

17 g of 6-methyltryptamine were dissolved at 40° C. under inert atmosphere in 500 ml of tetrahydrofuran, and the solution was allowed to return to ambient temperature. 14.6 ml of 1,5-diaza[5,4,0]undec-5-ene were added followed by 6.2 ml of chloroacetonitrile and stirring for 15 hours. The solvent was eliminated under reduced pressure and the residue was taken up in 250 ml of methylene chloride, washed with water, dried and concentrated to dryness. The 25 g of crude product was purified by chromatography on silica (eluent: methylene chloride-ethyl acetate 3-7) to obtain 13.2 g of the expected product melting at 92° C.

後処理

  1. customto return to ambient temperature
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated to dryness
  5. customThe 25 g of crude product was purified by chromatography on silica (eluent: methylene chloride-ethyl acetate 3-7)

出典と根拠

ORDレコード
ord-18c2620c8e904afd9387c033a505751a
出典データセット
uspto-grants-1989_12
特許番号
US04886802

反応ノート

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