Formaldehyde → HCID 22346322, 화합물

HRID 897342노트

반응식

HRID 897342 반응식
[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]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 122488Acetic acid, 2-methylhydrazideHCID 22346306HCID 22346306, 화합물

생성물 1

HCID 22346322HCID 22346322, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-cea68d1b2e0d44f094406927c8188d52
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06921759B2

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