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Diisopropylethylamine → Methyl 1-({(3S)-3-[(tert-butoxycarbonyl)amino]-3-phenylpropyl}amino)cyclopentanecarboxylate

HRID 1367218
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HRID 1367218 반응식
O=[CH:2][CH2:3][C@H:4]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.[NH2:20][C:21]1([C:26]([O:28][CH3:29])=[O:27])[CH2:25][CH2:24][CH2:23][CH2:22]1.CCN(C(C)C)C(C)C.C([O-])(O)=O.[Na+]>C(Cl)(Cl)Cl.O>[C:14]([O:13][C:12]([NH:11][C@H:4]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH2:3][CH2:2][NH:20][C:21]1([C:26]([O:28][CH3:29])=[O:27])[CH2:25][CH2:24][CH2:23][CH2:22]1)=[O:18])([CH3:17])([CH3:16])[CH3:15]
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참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 516892Sodium Bicarbonate2회HCID 11513856Methyl 1-amino-1-cyclopentanecarboxylate, HClHCID 11817535Boc-(S)-3-Amino-3-phenylpropanal

생성물 1

HCID 66973463Methyl 1-({(3S)-3-[(tert-butoxycarbonyl)amino]-3-phenylpropyl}amino)cyclopentanecarboxylate

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6212Chloroform용매

실험 절차

To a solution of tert-butyl [(1S)-3-oxo-1-phenylpropyl]carbamate from Step B (0.820 g, 3.29 mmol) and methyl 1-aminocyclopentanecarboxylate hydrochloride (0.591 g, 3.29 mmol) in chloroform (33 mL) was added Hunig's base (0.574 mL, 3.29 mmol). After stirring at ambient temperature for 20 min, NaHB(OAc)3 (1.74 g, 8.22 mmol) was added as a solid. Upon completion of the reaction, saturated aqueous NaHCO3 (3 mL) was added and the mixture was allowed to stir for at least 2 h. Water (5 mL) and additional saturated NaHCO3 (3 mL) was then added to form two layers. The aqueous layer was extracted once with chloroform (50 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo to give an oil. This oil was purified by silica gel chromatography, eluting with a gradient of MeOH:DCM 1:99 to 6:94, to give the title compound. MS: m/z=377 (M+1).

후처리

  1. additionwas added
  2. stirringto stir for at least 2 h
  3. customto form two layers
  4. extractionThe aqueous layer was extracted once with chloroform (50 mL)
  5. dry with materialThe combined organic layers were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customto give an oil
  9. customThis oil was purified by silica gel chromatography
  10. washeluting with a gradient of MeOH:DCM 1:99 to 6:94

출처 및 근거

ORD 기록
ord-141fcb0f02044f399eb9051b3f2a2776
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893079B2

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