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Dimethylformamide → 2-amino-4-phenylphthalazin-1(2H)-one

HRID 469534
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HRID 469534 반응식
[C:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:17])[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CC([O-])(C)C.[K+].C[N:25](C=O)C.C1(P(ON)(C2C=CC=CC=2)=O)C=CC=CC=1>CCOC(C)=O>[NH2:25][N:9]1[N:8]=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:17]
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참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 2191504-Phenyl-1-(2H)-phthalazinoneHCID 10955453O-(Diphenylphosphinyl)hydroxylamineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 212625372-amino-4-phenylphthalazin-1(2H)-one수율 95%

시약·촉매·용매 1

HCID 8857
Ethyl Acetate
용매

실험 절차

A mixture of 4-phenylphthalazin-1(2H)-one (Aldrich) (500 mg, 2.25 mmol) and KOtBu (3.37 mL, 3.37 mmol) was stirred for 45 minutes, diluted with DMF for solubility, and Example 17A (787 mg, 3.37 mmol) was added and stirred for 3 hours. The mixture was diluted with EtOAc, washed with saturated NaHCO3 and brine, dried (Na2SO4), filtered, and concentrated to give 509 mg (95%) of the title compound. MS (DCI/NH3) m/z 238 (M+H)+.

후처리

  1. additionwas added
  2. stirringstirred for 3 hours
  3. washwashed with saturated NaHCO3 and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8c387b1a38c74ff5b40ca8df2d698c73
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629143B2

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