Water → HCID 15733250, 화합물

HRID 2397575노트

반응식

HRID 2397575 반응식
[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

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 21436045HCID 21436045, 화합물

생성물 1

HCID 15733250HCID 15733250, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b3a2bf8524284c32bd212dda3ff87acc
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04022778

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