Nitrogen → HCID 44461420, 화합물

HRID 2268845노트

반응식

HRID 2268845 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 44461420HCID 44461420, 화합물수율 80%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2d5fe0357add43efafcf7a9be51c6a13
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329370B1

반응 노트

불러오는 중…