Picolyl chloride hydrochloride → HCID 19088785、化合物

HRID 1463922ノート

反応式

HRID 1463922 の反応式
[N:1]1([C:7]2[O:8][C:9]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)=[CH:10][C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[H-].[Na+].Cl.[N:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH2:30]Cl>CN(C)C=O>[N:1]1([C:7]2[O:8][C:9]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:30][C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][N:24]=4)=[CH:16][CH:15]=3)=[CH:10][C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 23392Picolyl chloride hydrochlorideHCID 24758Sodium hydrideHCID 97955054H-Pyran-4-one, 2-(4-hydroxyphenyl)-6-(4-morpholinyl)-

生成物 1

HCID 19088785HCID 19088785、化合物収率 34%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
55 °C

実験手順

2-Morpholinyl-6-(4-hydroxyphenyl)-4-pyrone, as prepared in Example 5, (273 mg, 1.0 mmole) was suspended in 6 ml dimethylformamide in a 25 ml one neck round bottom flask under nitrogen. The suspension was treated with sodium hydride suspension (192 mg, 4.0 mmole) and the reaction mixture was warmed to 55° C. for 40 minutes. The reaction was treated with 2-picolyl chloride hydrochloride (492 mg, 3.0 mmole) and the mixture was stirred 4 hours at 55° C. The reaction was poured into 50 ml 2N sodium hydroxide/ice and the precipitated solid was collected, washed with water and diethyl ether and was dried (188 mg). The crude material was recrystallized from ethyl acetate to give 123 mg (34%) of Compound 6 as an off-white solid.

後処理

  1. customthe precipitated solid was collected
  2. washwashed with water and diethyl ether
  3. customwas dried (188 mg)
  4. customThe crude material was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-9a0c7c3100b44115923226bcf8ae755b
出典データセット
uspto-grants-1994_04
特許番号
US05302613

反応ノート

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