5-Hydroxy-2-pentanone → HCID 21449343、化合物

HRID 597057

反応式

HRID 597057 の反応式
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([N:13]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)N=CC)=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.[OH:25][CH2:26][CH2:27][CH2:28][C:29](=O)[CH3:30]>C(O)C>[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([N:13]3[C:17]4[C:22](=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=4)[C:28]([CH2:27][CH2:26][OH:25])=[C:29]3[CH3:30])=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 140665-Hydroxy-2-pentanoneHCID 86734555acetaldehyde N1-(7-chloroquinazolin-4-yl)p-methoxyphenylhydrazone hydrochloride

生成物 1

HCID 21449343HCID 21449343、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of acetaldehyde N1 -(7-chloroquinazolin-4-yl)p-methoxyphenylhydrazone hydrochloride (3.2g.) and 5-hydroxy-pentane-2-one (1.1g.) in ethanol (60ml.) was refluxed for 18 hours. The mixture was cooled and filtered and the filtrate evaporated in vacuo. The residue was chromatographed on silica gel (100g.) using, as eluant, petroleum ether (b.p. 40° -60° C.) containing an increasing proportion of ether (polarity increased by incremental addition of 10% v/v ether) to give 1-(7-chloroquinazolin-4-yl)-3-(2-hydroxyethyl)-5-methoxy-2-methylindole, m.p. 148°-150° C.

後処理

  1. temperatureThe mixture was cooled
  2. filtrationfiltered
  3. customthe filtrate evaporated in vacuo
  4. customThe residue was chromatographed on silica gel (100g.)
  5. additionpetroleum ether (b.p. 40° -60° C.) containing an increasing proportion of ether (polarity increased by incremental addition of 10% v/v ether)

出典と根拠

ORDレコード
ord-4cd57e6b87b44399bb594949dd5a8a41
出典データセット
uspto-grants-1977_03
特許番号
US04012513

関連ノート

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