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3-(Trifluoromethoxy)benzylamine → 4-chloro-7-(3-trifluoromethoxy-benzylamino)-2H-phthalazin-1-one

HRID 1667462
ノート
印刷プレビュー

反応式

HRID 1667462 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[NH:7][N:6]=[C:5]2[Cl:13].BrC1C=C2C(C(Cl)=NNC2=O)=CC=1.[F:27][C:28]([F:39])([F:38])[O:29][C:30]1[CH:31]=[C:32]([CH:35]=[CH:36][CH:37]=1)[CH2:33][NH2:34].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC([O-])(C)C.[Na+]>CC(N(C)C)=O.CCOC(C)=O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:13][C:5]1[C:4]2[C:9](=[CH:10][C:11]([NH:34][CH2:33][C:32]3[CH:35]=[CH:36][CH:37]=[C:30]([O:29][C:28]([F:27])([F:38])[F:39])[CH:31]=3)=[CH:2][CH:3]=2)[C:8](=[O:12])[NH:7][N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 1452643-(Trifluoromethoxy)benzylamineHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 533084876-Bromo-4-chlorophthalazin-1(2H)-oneHCID 674169997-bromo-4-chloro-2H-phthalazin-1-one

生成物 1

HCID 584473154-chloro-7-(3-trifluoromethoxy-benzylamino)-2H-phthalazin-1-one

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 8857Ethyl Acetate溶媒HCID 31374Dimethylacetamide溶媒

実験手順

A mixture 6-bromo-4-chloro-2H-phthalazin-1-one and 7-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.58 mmol), 3-(trifluoromethoxy)benzylamine (0.08 mL, 0.636 mmol), Pd2(dba)3 (61 mg, 0.0667 mmol), rac-BINAP (120 mg, 0.193 mmol) and NaOt-Bu (155 mg, 1.613 mmol) in DMA (8 mL) was heated at 80° C. for 1 h. The mixture was allowed to cool. The mixture was allowed to cool, diluted with EtOAc and washed with water. The organic layer was washed with sat.aq. NaHCO3, brine and dried (Na2SO4). Chromatography on silica (EtOAc/hexanes) afforded 4-chloro-7-(3-trifluoromethoxy-benzylamino)-2H-phthalazin-1-one (28 mg) as an off white solid, 1H (600 MHz, CDCl3) δ: 4.50 (s, 2H), 7.06 (dd, 1H), 7.14 (d, 1H), 7.18 (s, 1H), 7.28 (d, 1H), 7.38 (t, 1H), 7.44 (d, 1H), 7.78 (d, 1H), 9.48 (s, 1H), m/z (M+1) 369.93; 4-chloro-6-(3-trifluoromethoxy-benzylamino)-2H-phthalazin-1-one (22 mg) as an off white solid, 1H (600 MHz, CDCl3) δ: 4.41 (s, 2H), 6.83 (d, 1H), 6.98 (dd, 1H), 7.08 (bd, 1H), 7.16 (bs, 1H), 7.25 (s, 1H), 7.32 (t, 1H), 8.06 (d, 1H), 10.15 (s, 1H) ppm. m/z (M+1) 369.93.

後処理

  1. temperatureto cool
  2. temperatureto cool
  3. washwashed with water
  4. washThe organic layer was washed with sat.aq
  5. dry with materialNaHCO3, brine and dried (Na2SO4)

出典と根拠

ORDレコード
ord-06f99a9f90af4afdb434e54e66d005ed
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044041B2

反応ノート

読み込み中…

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