Formaldehyde → HCID 22346322、化合物

HRID 897342ノート

反応式

HRID 897342 の反応式
[CH3:1][O:2][C:3]1[CH:26]=[CH:25][C:6]([CH2:7][O:8][C:9]2[C:10]([C:21]([O:23][CH3:24])=[O:22])=[N:11][C:12]([CH:19]=[CH2:20])=[C:13]3[C:18]=2[N:17]=[CH:16][CH:15]=[CH:14]3)=[CH:5][CH:4]=1.[CH2:27]=O.[C:29]([NH:32][NH:33][CH3:34])(=[O:31])[CH3:30]>C1(C)C=CC=CC=1>[C:29]([N:32]1[CH:19]([C:12]2[N:11]=[C:10]([C:21]([O:23][CH3:24])=[O:22])[C:9]([O:8][CH2:7][C:6]3[CH:25]=[CH:26][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)=[C:18]3[C:13]=2[CH:14]=[CH:15][CH:16]=[N:17]3)[CH2:20][CH2:34][N:33]1[CH3:27])(=[O:31])[CH3:30]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 122488Acetic acid, 2-methylhydrazideHCID 22346306HCID 22346306、化合物

生成物 1

HCID 22346322HCID 22346322、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

A mixture of methyl 8-[(4-methoxybenzyl)oxy]-5-vinyl-[1,6]-naphthyridine-7-carboxylate (0.26 g, 0.73 mmol), paraformaldehyde (96 mg), and 1-acetyl-2-methylhydrazine (0.22 g, 2.45 mmol; J. Org. Chem. 1972, 37, 3608) in toluene (15 mL) was heated in an oil bath at 120° C. for 1.5 hour. The resulting mixture was concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting first with a gradient of 0-5% methanol in ethyl acetate. Collection and concentration of appropriate fractions provided the title acetylpyrazolidine.

後処理

  1. concentrationThe resulting mixture was concentrated under vacuum
  2. customCollection and concentration of appropriate fractions

出典と根拠

ORDレコード
ord-cea68d1b2e0d44f094406927c8188d52
出典データセット
uspto-grants-2005_07
特許番号
US06921759B2

反応ノート

読み込み中…