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m-Chloroperbenzoic acid → HCID 178479968, 화합물

HRID 511554
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HRID 511554 반응식
[NH2:1][C:2]1[C:7]2[C:8](=[O:12])[N:9]([CH3:11])[CH2:10][C:6]=2[CH:5]=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:21])C=1>CC(C)=O>[NH2:1][C:2]1[C:7]2[C:8](=[O:12])[N:9]([CH3:11])[CH2:10][C:6]=2[CH:5]=[CH:4][N+:3]=1[O-:21]
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4

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HCID 70297m-Chloroperbenzoic acidHCID 672535394-amino-2-methyl-1,2-dihydro-3H-pyrrolo[3,4-c]pyridin-3-one2회

생성물 1

HCID 178479968HCID 178479968, 화합물수율 99.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 4-amino-2-methyl-1,2-dihydro-3H-pyrrolo[3,4-c]pyridin-3-one (Compound 3108, 62.5 mg, 0.383 mmol) and m-Chloroperbenzoic acid (145 mg, 0.843 mmol) in Acetone (10.0 mL) was stirred at rt for 90 minutes. The reaction mixture was concentrated under reduced pressure to an off white solid. The crude material was purified by silica gel chromatography on the combi-flash Rf system using DCM/7 N NH3 in MeOH (100:0→90:10) as eluent. The fractions containing product were combined and concentrated under reduced pressure to yield a white solid (68.3 mg, 99.5%). 1H NMR (DMSO-d6, 400 MHz): δ=8.19 (d, J=6.57 Hz, 1H), 7.02 (br. s., 2H), 6.82 (d, J=6.57 Hz, 1H), 4.41 (s, 2H), 3.01 (s, 3H). MS (ES+): m/z 180.07 [MH+] (TOF, polar).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure to an off white solid
  2. customThe crude material was purified by silica gel chromatography on the combi-flash Rf system
  3. additionThe fractions containing product
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-600c9f62e08349149923aa25f65a5772
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096624B2

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