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N,N,N',N'-Tetramethylethylenediamine → benzyl (2S)-2-[(4-{(1S)-1-[(tert-butoxycarbonyl)amino]ethyl}phenyl)(hydroxy)methyl]-2-methylpyrrolidine-1-carboxylate

HRID 1010914
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HRID 1010914 반응식
[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]([C:10]1[CH:15]=[CH:14][C:13](Br)=[CH:12][CH:11]=1)[CH3:9])([CH3:4])([CH3:3])[CH3:2].CN(C)CCN(C)C.C([Li])CCC.[CH:31]([C@:33]1([CH3:48])[CH2:37][CH2:36][CH2:35][N:34]1[C:38]([O:40][CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)=[O:39])=[O:32].[Cl-].[NH4+]>O1CCCC1>[C:1]([O:5][C:6]([NH:7][C@H:8]([C:10]1[CH:15]=[CH:14][C:13]([CH:31]([OH:32])[C@:33]2([CH3:48])[CH2:37][CH2:36][CH2:35][N:34]2[C:38]([O:40][CH2:41][C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[O:39])=[CH:12][CH:11]=1)[CH3:9])=[O:17])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

7

반응물 5

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 25517Ammonium ChlorideHCID 56973617(S)-tert-Butyl (1-(4-bromophenyl)ethyl)carbamateHCID 86625219benzyl (2S)-2-formyl-2-methylpyrrolidine-1-carboxylateHCID 178418339Butyllithium

생성물 1

HCID 67312882
benzyl (2S)-2-[(4-{(1S)-1-[(tert-butoxycarbonyl)amino]ethyl}phenyl)(hydroxy)methyl]-2-methylpyrrolidine-1-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

423 mg of the compound [1-1] and 508 mg of N,N,N′,N′-tetramethylethylene diamine were dissolved in 22 mL of tetrahydrofuran, the temperature of the solution was kept at −78° C., and then 1.09 mL of n-butyl lithium (2.66 M hexane solution) was added thereto. After stirring at the same temperature for 1 hour to obtain the resultant white suspension, 2.2 mL of a tetrahydrofuran solution prepared by dissolving 384 mg of the compound [63-3] was added thereto, and the mixture was stirred at the same temperature for 1.5 hours. To the reaction mixture, a saturated aqueous ammonium chloride solution was added, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. Thereafter, the insolubles were filtered, and the filtrate was concentrated under reduced pressure to obtain benzyl (2S)-2-[(4-{(1S)-1-[(tert-butoxycarbonyl)amino]ethyl}phenyl)(hydroxy)methyl]-2-methylpyrrolidine-1-carboxylate [634]. The compound [634] obtained was a mixture of two isomers, which was then purified by silica gel column chromatography (eluent: hexane/ethyl acetate=100/0 to 40/60) to obtain 199 mg of a low polarity compound (compound that eluted first under the above condition) [634a] (hereinafter, referred to as the compound [634a]) and 117 mg of a high polarity compound (compound that eluted afterwards under the above condition) [634b] (hereinafter, referred to as the compound [63-4b]). Here, the compound [634a] is a precursor of a compound [63], and the compound [634b] is a precursor of a compound [64] described later.

후처리

  1. customwas kept at −78° C.
  2. customprepared
  3. additionwas added
  4. stirringthe mixture was stirred at the same temperature for 1.5 hours
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe obtained organic layer was washed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationThereafter, the insolubles were filtered
  9. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-47c66fec86324c45bfb2da22c7a44b4d
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977336B2

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