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Diisopropylamine → HCID 70050443, 화합물

HRID 1720488
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HRID 1720488 반응식
C(NC(C)C)(C)C.[C:8]1([CH3:17])[CH:13]=[CH:12][C:11]([S@:14]([CH3:16])=[O:15])=[CH:10][CH:9]=1.[CH2:18]([O:25][C:26]([N:28]1[CH2:41][CH2:40][CH2:39][C@H:29]1[C:30]([N:32]1[CH2:38][CH2:37][CH2:36][C@H:33]1[CH:34]=[O:35])=[O:31])=[O:27])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[Cl-].[NH4+]>C1COCC1>[CH2:18]([O:25][C:26]([N:28]1[CH2:41][CH2:40][CH2:39][C@H:29]1[C:30]([N:32]1[CH2:38][CH2:37][CH2:36][C@H:33]1[CH:34]([OH:35])[CH2:16][S@@:14]([C:11]1[CH:12]=[CH:13][C:8]([CH3:17])=[CH:9][CH:10]=1)=[O:15])=[O:31])=[O:27])[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7912DiisopropylamineHCID 25517Ammonium ChlorideHCID 122623Benzyl 2-(2-formylpyrrolidine-1-carbonyl)pyrrolidine-1-carboxylateHCID 11170275(S)-(-)-Methyl p-tolyl sulfoxide

생성물 1

HCID 70050443HCID 70050443, 화합물수율 88.2%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

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온도
0 °C

실험 절차

To diisopropylamine (0.26 ml) in THF (6 ml) was dropwise added 1.62M n-butyllithium-hexane solution (1.12 ml) at -78° C., and the mixture was stirred at 0° C. for 0.5 hour. The reaction mixture was cooled to -30° C., dropwise added with (S)-(-)-methyl p-tolyl sulfoxide (255 mg) in THF (6 ml), and stirred at 0° C. for 0.5 hour. The reaction mixture was cooled to -78° C. and dropwise added with known N-benzyloxycarbonyl-L-prolyl-L-prolinal (300 mg) in THF (6 ml). After stirring for 0.5 hour, an aqueous solution of saturated ammonium chloride was added thereto, followed by stirring at room temperature for 10 minutes. The reaction mixture was extracted with ethyl acetate, and the organic layer was washed with a saturated aqueous solution of sodium bicarbonate and saturated brine order, dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (eluate; chloroform-methanol) to give 388 mg of the title compound.

후처리

  1. customat -78° C.
  2. temperatureThe reaction mixture was cooled to -30° C.
  3. stirringstirred at 0° C. for 0.5 hour
  4. temperatureThe reaction mixture was cooled to -78° C.
  5. stirringAfter stirring for 0.5 hour
  6. stirringby stirring at room temperature for 10 minutes
  7. extractionThe reaction mixture was extracted with ethyl acetate
  8. washthe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and saturated brine order
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated
  11. customThe residue was purified by silica gel column chromatography (eluate; chloroform-methanol)

출처 및 근거

ORD 기록
ord-3e6f706c851e499eb3d97ef7385fee51
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05506256

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