Potassium Hydroxide → Ihch-7113

HRID 629316노트

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HRID 629316 반응식
[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]3[C@@H:12]4[CH2:17][N:16](C(OCC)=O)[CH2:15][CH2:14][C@@H:13]4[N:5]([C:6]=23)[CH2:4][CH2:3]1.[OH-].[K+]>C(O)CCC>[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]3[C@@H:12]4[CH2:17][NH:16][CH2:15][CH2:14][C@@H:13]4[N:5]([C:6]=23)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 21302624Ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-3-methyl-1H-pyrido(3',4':4,5)pyrrolo(1,2,3-de)quinoxaline-8(7H)-carboxylate

생성물 1

HCID 21302499Ihch-7113

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
120 °C

실험 절차

Ethyl(6bR,10aS)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido-[3′,4′:4,5]-pyrrolo[1,2,3-de]quinoxaline-8-carboxylate (ca. 18.5 g, 57 mmol), KOH (12.7 g, 226 mmol) and n-butanol are placed in a 300 ml pressure bottle and heated in an oil bath at 120° C. for 3 hours. n-butanol is removed in vacuo and 300 ml of water is added and then extracted with DCM. The DCM layers are combined and washed with brine and dried (Na2SO4). Evaporation of the solvent gives (6bR,10aS)-3-methyl-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido-[3′,4′:4,5]-pyrrolo[1,2,3-de]quinoxaline.

후처리

  1. customn-butanol is removed in vacuo and 300 ml of water
  2. additionis added
  3. extractionextracted with DCM
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-3d3db8fb8b484203bad9ba6b642095cd
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315504B2

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