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Hydrochloric Acid → methyl 13-cyclohexyl-6-(hydroxymethyl)-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-10-carboxylate

HRID 421965
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HRID 421965 반응식
[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:29]([O:31][CH3:32])=[O:30])=[CH:12][C:13]=3[N:14]3[CH2:20][CH:19]([C:21](OC)=[O:22])[CH2:18][C:17]4[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=4[C:15]=23)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Li+].[BH4-].O.Cl>C1COCC1>[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:29]([O:31][CH3:32])=[O:30])=[CH:12][C:13]=3[N:14]3[CH2:20][CH:19]([CH2:21][OH:22])[CH2:18][C:17]4[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=4[C:15]=23)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
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6

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HCID 313Hydrochloric AcidHCID 962WaterHCID 4148881Lithium borohydrideHCID 58765149dimethyl 13-cyclohexyl-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-6,10-dicarboxylate

생성물 1

HCID 16072734methyl 13-cyclohexyl-6-(hydroxymethyl)-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-10-carboxylate수율 85%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

Dimethyl 13-cyclohexyl-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-6,10-dicarboxylate (prepared according to International patent application publication WO 2006/020082) was dissolved in anhydrous THF (0.02 M) and after cooling at 0° C. BH3THF complex (1.5 eq.) was added followed by LiBH4 (1 eq.) and water (4 eq.). The mixture was left stirring at RT for 2h, then 1N hydrochloric acid was slowly added. The crude was extracted twice with EtOAc, dried over Na2SO4, filtered, and all volatiles were removed in vacuo to obtain desired compound as a yellow solid (85%) that was used in the next step without purification. (ES+) m/z 404 (M+H)+.

후처리

  1. additionBH3THF complex (1.5 eq.) was added
  2. waitThe mixture was left
  3. extractionThe crude was extracted twice with EtOAc
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customall volatiles were removed in vacuo

출처 및 근거

ORD 기록
ord-1b52f181c0f9412180590557b9e1ceaa
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101595B2

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