Diisopropylethylamine → 4,6-Dimethoxy-2-(alpha-fluorobenzyl) pyrimidine

HRID 1440962ノート

反応式

HRID 1440962 の反応式
Cl.Cl.[C:3](=[NH:11])([O:9][CH3:10])[CH2:4][C:5](=[NH:8])[O:6][CH3:7].C(N(C(C)C)C(C)C)C.[F:21][CH:22]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:23](Cl)=O>ClCCl>[CH3:7][O:6][C:5]1[CH:4]=[C:3]([O:9][CH3:10])[N:11]=[C:23]([CH:22]([F:21])[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:8]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 12896693Dimethyl malonimidate dihydrochlorideHCID 149495282-Fluoro-2-phenylacetyl chloride

生成物 1

HCID 541012184,6-Dimethoxy-2-(alpha-fluorobenzyl) pyrimidine収率 103.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

Dimethyl malonimidate dihydrochloride (11.0 g) was suspended in dichloromethane (100 ml) at -40° C. Ethyl diisopropylamine (38.9 ml) was added dropwise over 15 minutes at -40° C., followed by 2-fluoro-2-phenylacetyl chloride (11.0 g) in dichloromethane (15 ml) over 10 minutes at -40° C. The reaction mixture was allowed to warm to room temperature and stand overnight. It was then diluted further with dichloromethane, washed with ammonium chloride solution, then with water, and was dried over magnesium sulfate. The dichloromethane solution was evaporated to dryness to give 13.9 g of the desired product.

後処理

  1. washwashed with ammonium chloride solution
  2. dry with materialwith water, and was dried over magnesium sulfate
  3. customThe dichloromethane solution was evaporated to dryness

出典と根拠

ORDレコード
ord-6138cea4710c432493891253a750fc80
出典データセット
uspto-grants-1996_03
特許番号
US05502028

反応ノート

読み込み中…