Nitrogen → HCID 44461420、化合物

HRID 2268845ノート

反応式

HRID 2268845 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[CH2:12][NH:11][N:10]=1.N#N.[O-:24][C:25]#[N:26].[K+].[OH-].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[CH2:12][N:11]([C:25]([NH2:26])=[O:24])[N:10]=1

参加物

6

反応物 4

HCID 947NitrogenHCID 14798Sodium HydroxideHCID 9797215Phthalazine, 4-[(3,5-dichloro-4-pyridinyl)methyl]-1,2-dihydro-7-methoxy-HCID 11378442Potassium cyanate

生成物 1

HCID 44461420HCID 44461420、化合物収率 80%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1,2-dihydro-phthalazine (0.4 g, 1.24 mmoles), prepared as described in example 22, in glacial acetic acid (8 ml), under stirring and dry N2 at room temperature, was added with potassium cyanate (0.2 g, 2.48 mmoles) and the reaction mixture was left to stand for 20 hours, then poured into 10% NaOH in excess and extracted more times with CH2Cl2. The organic phases were washed with water, anhydrified and concentrated to give a residue which was flash chromatographed (eluent: hexane/ethyl acetate 3:7) to give 0.36 g of the title compound (yield: 80%). m.p.>230° C.

後処理

  1. waitthe reaction mixture was left
  2. extractionextracted more times with CH2Cl2
  3. washThe organic phases were washed with water, anhydrified
  4. concentrationconcentrated
  5. customto give a residue which
  6. customchromatographed (eluent: hexane/ethyl acetate 3:7)

出典と根拠

ORDレコード
ord-2d5fe0357add43efafcf7a9be51c6a13
出典データセット
uspto-grants-2001_12
特許番号
US06329370B1

反応ノート

読み込み中…