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Sodium Hydroxide → 6-(6,7-Dimethoxy-quinolin-4-ylmethyl)-naphthalen-2-ylamine

HRID 2115774
ノート
印刷プレビュー

反応式

HRID 2115774 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([CH2:12][C:13]1[C:22]3[C:17](=[CH:18][C:19]([O:25][CH3:26])=[C:20]([O:23][CH3:24])[CH:21]=3)[N:16]=[CH:15][CH:14]=1)[CH:6]=[CH:5]2.P(C(C)(C)C)(C(C)(C)C)C(C)(C)C.[Li+].C[Si]([N-:45][Si](C)(C)C)(C)C.[OH-].[Na+]>CCOCC.Cl.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].C1(C)C=CC=CC=1>[CH3:24][O:23][C:20]1[CH:21]=[C:22]2[C:17](=[CH:18][C:19]=1[O:25][CH3:26])[N:16]=[CH:15][CH:14]=[C:13]2[CH2:12][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[CH:3]=[C:2]([NH2:45])[CH:11]=[CH:10]2
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 4

HCID 14798Sodium HydroxideHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 2733832Lithium HexamethyldisilazideHCID 67520211HCID 67520211、化合物

生成物 1

HCID 675205706-(6,7-Dimethoxy-quinolin-4-ylmethyl)-naphthalen-2-ylamine

試薬・触媒・溶媒 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 313Hydrochloric Acid溶媒
HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒

実験手順

To a sealed tube, 4-(6-bromo-naphthalen-2-ylmethyl)-6,7-dimethoxy-quinoline (Step f, 100 mg, 0.11 mmol), Pd2(dba)3 (5 mg, 0.0055 mmol), P(t-Bu)3 (1.1 mg, 0.0055 mmol), toluene (1 mL) was combined under nitrogen, followed by addition of LiHMDS (1M in THF, 0.137 mL, 0.137 mmol). The reaction was stirred at RT overnight. The suspension was diluted with Et2O and HCl (1M, 1 mL) was added. The crude material was poured into 1N NaOH and extracted with Et2O 3×. The combined organic layer was washed with water and brine, dried on Na2SO4, filtered, concentrated and purified by prep-TLC with 100% EtOAc to give the desired compound. MS (ESI, pos. ion) m/z: 345.1 (M+1).

後処理

  1. additionwas added
  2. extractionextracted with Et2O 3×
  3. washThe combined organic layer was washed with water and brine
  4. customdried on Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by prep-TLC with 100% EtOAc

出典と根拠

ORDレコード
ord-f496066638944e839ef66c8417b2d1d5
出典データセット
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07435823B2

反応ノート

読み込み中…

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