5-Chloro-2(1H)-pyrimidinone → HCID 12791252、化合物

HRID 1906158ノート

反応式

HRID 1906158 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.Br[CH2:10][C:11]([C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[NH:15][CH:14]=1)=[O:12]>C(N(CC)CC)C.C(O)C>[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[N:6]([CH2:10][C:11]([C:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[NH:15][CH:14]=2)=[O:12])[CH:7]=1

参加物

5

反応物 2

HCID 1085785-Chloro-2(1H)-pyrimidinoneHCID 113109362-bromo-1-(1H-indol-3-yl)ethanone

生成物 1

HCID 12791252HCID 12791252、化合物収率 57.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8471Triethylamine溶媒

実験手順

A mixture of 5-chloropyrimidin-2-one (522 mg) and 3-bromoacetylindole (1.19 g) in triethylamine (0.84 ml) and ethanol (25 ml) was stirred at room temperature. After 1.5 h the mixture was heated to 55° C. After a further 1.5 h the mixture was cooled and the resulting precipitate collected and washed with cold ethanol. Recrystallisation twice from ethyl acetate and once from ethanol gave the title pyrimidinone (660 mg), m.p. 228°-229° C., λmax (EtOH) 240 nm (ε 16,370) 300.5 nm (ε 13,090).

後処理

  1. temperatureAfter 1.5 h the mixture was heated to 55° C
  2. temperatureAfter a further 1.5 h the mixture was cooled
  3. customthe resulting precipitate collected
  4. washwashed with cold ethanol
  5. customRecrystallisation twice from ethyl acetate

出典と根拠

ORDレコード
ord-ab83a1a35df74ae5b92aa9bbb23a3478
出典データセット
uspto-grants-1987_03
特許番号
US04650800

反応ノート

読み込み中…