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Nitrogen → 1-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-4-morpholin-4-yl-phthalazine

HRID 2268883
ノート
印刷プレビュー

反応式

HRID 2268883 の反応式
N#N.Cl[C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([O:14][CH3:15])[CH:12]=2)[C:7]([CH2:16][C:17]2[C:22]([Cl:23])=[CH:21][N:20]=[CH:19][C:18]=2[Cl:24])=[N:6][N:5]=1.[NH:25]1[CH2:30][CH2:29][O:28][CH2:27][CH2:26]1.CCCCCC.C(OCC)(=O)C>CN(C=O)C>[Cl:24][C:18]1[CH:19]=[N:20][CH:21]=[C:22]([Cl:23])[C:17]=1[CH2:16][C:7]1[C:8]2[C:13](=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)[C:4]([N:25]2[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)=[N:5][N:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 947NitrogenHCID 8083MorpholineHCID 186292104-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazineHCID 21226206Ethyl acetate hexane

生成物 1

HCID 99092171-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-4-morpholin-4-yl-phthalazine収率 79%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
100 °C

実験手順

A solution under stirring and dry N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (1 g, 2.82 mmoles), prepared as described in example 45, in DMF (25 ml), at room temperature, was added with morpholine (0.73 g, 8.46 mmoles) and the temperature was raised to 100° C. After 14 hours the whole was brought to dryness and the solid partitioned between water and CH2Cl2. The organic phase was washed with water, anhydrified and brought to dryness to give a solid which was flash chromatographed (eluent: hexane/ethyl acetate 6:4, then in gradient up to 3:7) to give 0.9 g of the title compound (yield: 79%). m.p.: 179-180° C.

後処理

  1. customthe solid partitioned between water and CH2Cl2
  2. washThe organic phase was washed with water
  3. customto give a solid which
  4. customchromatographed (eluent

出典と根拠

ORDレコード
ord-3dabbd2e8c80456fbad1280df027890e
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329370B1

反応ノート

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