Sodium hydride → HCID 22639999、化合物

HRID 2415098

反応式

HRID 2415098 の反応式
[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([CH3:9])[N:5]=[C:4]([CH3:10])[N:3]=1.[CH2:11]([O:18][C:19]1[CH:20]=[C:21]([CH:24]=[CH:25][C:26]=1[O:27][CH3:28])[CH2:22]Cl)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[H-].[Na+]>CN1CCCC1=O>[CH2:11]([O:18][C:19]1[CH:20]=[C:21]([CH:24]=[CH:25][C:26]=1[O:27][CH3:28])[CH2:22][NH:1][C:2]1[C:7]([Cl:8])=[C:6]([CH3:9])[N:5]=[C:4]([CH3:10])[N:3]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 2802242-(Benzyloxy)-4-(chloromethyl)-1-methoxybenzeneHCID 5938434-Amino-5-chloro-2,6-dimethylpyrimidine

生成物 1

HCID 22639999HCID 22639999、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

In analogy to the method described in example A1, 6.11 g (38 mmol) of 4-amino-5-chloro-2,6-dimethylpyrimidine, 10.5 g (40 mmol) of 3-benzyloxy-4-methoxybenzyl chloride and 1.52 g (38 mmol) of sodium hydride (60% suspension in liquid paraffin) are reacted in a total of 225 ml of N-methylpyrrolidone. After chromatography on silica gel (mobile phase: toluene/dioxane=10:1) and crystallization from petroleum ether, the title compound is isolated as a pale beige solid. Yield: 5.2 g (36% of theory). m.p.: 111-117° C.

後処理

  1. customAfter chromatography on silica gel (mobile phase: toluene/dioxane=10:1) and crystallization from petroleum ether

出典と根拠

ORDレコード
ord-da5ef040252f4ae794caf6685df07b0d
出典データセット
uspto-grants-2004_11
特許番号
US06818642B2

関連ノート

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