Water → HCID 15733250、化合物

HRID 2397575ノート

反応式

HRID 2397575 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:16]=[CH:15][C:14]2[N:13]3[CH2:17][CH2:18][NH:19][C:20](=O)[C:12]3=[C:11]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:10]=2[CH:9]=1.O>O1CCCC1>[Cl:7][C:8]1[CH:16]=[CH:15][C:14]2[N:13]3[CH2:17][CH2:18][NH:19][CH2:20][C:12]3=[C:11]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:10]=2[CH:9]=1

参加物

5

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 21436045HCID 21436045、化合物

生成物 1

HCID 15733250HCID 15733250、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred solution of lithium aluminum hydride (1 gram, 0.026 mole) in 20 ml dry tetrahydrofuran (THF) is added slowly a suspension of 1,2,3,4-tetrahydro-8-chloro-10-phenylpyrazino[1,2-a] indole-1-one (5.2 grams, 0.018 mole) in 40 ml of dry THF. This reaction mixture is stirred and refluxed for 8 hours after which it is cooled and decomposed by the slow addition of 3 ml of water. After stirring 1 hour the suspension is filtered. The filtercake is washed with isopropanol, THF, and acetone. The combined filtrate is taken to dryness and recrystallized from ethanol. The product is filtered off, washed with ether, and dried. The above titled product has a m.p. 163°-64° C. yield 4.5 grams (90%).

後処理

  1. temperaturerefluxed for 8 hours after which it
  2. temperatureis cooled
  3. stirringAfter stirring 1 hour the suspension
  4. filtrationis filtered
  5. washThe filtercake is washed with isopropanol, THF, and acetone
  6. customrecrystallized from ethanol
  7. filtrationThe product is filtered off
  8. washwashed with ether
  9. customdried

出典と根拠

ORDレコード
ord-b3a2bf8524284c32bd212dda3ff87acc
出典データセット
uspto-grants-1977_05
特許番号
US04022778

反応ノート

読み込み中…