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HCID 45739920, 화합물 → HCID 58654344, 화합물

HRID 1170525
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HRID 1170525 반응식
C(OC([N:8]1[CH2:12][CH2:11][CH2:10][CH:9]1[C:13](=[O:25])[NH:14][CH2:15][C:16]1[CH:24]=[CH:23][C:19]2[O:20][CH2:21][O:22][C:18]=2[CH:17]=1)=O)(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[O:20]1[C:19]2[CH:23]=[CH:24][C:16]([CH2:15][NH:14][C:13]([CH:9]3[CH2:10][CH2:11][CH2:12][NH:8]3)=[O:25])=[CH:17][C:18]=2[O:22][CH2:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 45739920HCID 45739920, 화합물

생성물 1

HCID 58654344HCID 58654344, 화합물수율 43%

시약·촉매·용매 1

HCID 21863450Trifluoroacetic acid methylene chloride용매

실험 절차

2-[(Benzo[1,3]dioxol-5-ylmethyl)-carbamoyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (278 mg, 0.80 mmol) was dissolved in DCM:TFA (1:1, 6 mL) and stirred at room temperature for 3 hours. After this period, the solution was concentrated down under vacuum. The crude material was diluted in DCM (50 mL) and washed with 1M NaOH (aq) (50 mL) to afford the crude residue. The crude product was purified by Flash chromatography (0-10% methanol/DCM gradient) to afford 85.1 mg (43%) of pyrrolidine-2-carboxylic acid (benzo[1,3]dioxol-5-ylmethyl)-amide. [M+H]+ 249.08.

후처리

  1. wait
After this period
  • concentrationthe solution was concentrated down under vacuum
  • additionThe crude material was diluted in DCM (50 mL)
  • washwashed with 1M NaOH (aq) (50 mL)
  • customto afford the crude residue
  • customThe crude product was purified by Flash chromatography (0-10% methanol/DCM gradient)
  • 출처 및 근거

    ORD 기록
    ord-f4ce68ebd12345a2851a37ea4566464b
    출처 데이터셋
    uspto-grants-2010_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07825256B2

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