Dimethylformamide → N-Cyclopropyl-3-(1-isopropylphthalazin-6-yl)-4-methylbenzamide

HRID 2357544ノート

反応式

HRID 2357544 の反応式
[CH:1]([C:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]3[CH:15]=[C:16]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:17]([OH:19])=O)=[CH:11][CH:12]=2)[CH:7]=[N:6][N:5]=1)([CH3:3])[CH3:2].CN(C(ON1N=NC2[CH:35]=[CH:36][CH:37]=[N:38]C1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN(C)C=O.C1(N)CC1>C(OCC)(=O)C>[CH:37]1([NH:38][C:17](=[O:19])[C:16]2[CH:20]=[CH:21][C:22]([CH3:23])=[C:14]([C:10]3[CH:9]=[C:8]4[C:13](=[CH:12][CH:11]=3)[C:4]([CH:1]([CH3:2])[CH3:3])=[N:5][N:6]=[CH:7]4)[CH:15]=2)[CH2:35][CH2:36]1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 69828CyclopropylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 684522933-(1-Isopropylphthalazin-6-yl)-4-methylbenzoic acid

生成物 1

HCID 68452802N-Cyclopropyl-3-(1-isopropylphthalazin-6-yl)-4-methylbenzamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A 10-mL round-bottom flask was charged with 3-(1-isopropylphthalazin-6-yl)-4-methylbenzoic acid (32 mg, 0.10 mmol), HATU (60 mg, 0.157 mmol), and N,N-dimethylformamide (0.5 mL), followed by cyclopropylamine (0.03 mL, 0.52 mmol). The resulting golden yellow mixture was stirred at RT for 18 h. The reaction mixture was diluted with ethyl acetate and washed with water and brine, then dried (MgSO4) and concentrated in vacuo. CombiFlash purification (20% to 70% ethyl acetate in Hexane) afforded the title compound as an off-white amorphous solid. MS (ES+): 346.2 (M+H)+.

後処理

  1. washwashed with water and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customCombiFlash purification (20% to 70% ethyl acetate in Hexane)

出典と根拠

ORDレコード
ord-73a52676640b4e7ba6c84383ea6ae339
出典データセット
uspto-grants-2010_07
特許番号
US07759337B2

反応ノート

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