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Hydrochloric Acid → HCID 178451481, 화합물

HRID 710468
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HRID 710468 반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][N:7]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:6]2)#[N:2].Cl.[NH2:20][OH:21].CCN(C(C)C)C(C)C>CCO>[OH:21][NH:20][C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][N:7]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:6]2)=[NH:2]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 787HydroxylamineHCID 81531DiisopropylethylamineHCID 18630967tert-Butyl 5-cyano-1,3-dihydro-2H-isoindole-2-carboxylate

생성물 1

HCID 178451481HCID 178451481, 화합물수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A product of Step C (0.22 g; 0.904 mmol), HCl×NH2OH (0.16 g; 2.3 mmol) and DIPEA (0.48 ml; 5 mmol) in anhydrous EtOH (3.5 ml) was refluxed for 2 h under N2. The solvents were removed under reduced pressure and the residue was diluted to 30 ml with EtOAc, washed with H2O (2×5 ml), brine, dried over anhydrous MgSO4, filtered and the filtrate evaporated to dryness to give the title compound (0.25 g; 100%) as colourless foam, which was used in next step without further purification.

후처리

  1. customThe solvents were removed under reduced pressure
  2. additionthe residue was diluted to 30 ml with EtOAc
  3. washwashed with H2O (2×5 ml), brine
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customthe filtrate evaporated to dryness

출처 및 근거

ORD 기록
ord-b59620437afd4f83861a8cb69e00ba44
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181182B2

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