Sodium Acetate → HCID 11630741, 화합물

HRID 2172151노트

반응식

HRID 2172151 반응식
[CH:1]([CH:3]([CH:13]=O)[C:4]1[N:9]=[C:8]([C:10]([OH:12])=[O:11])[CH:7]=[CH:6][CH:5]=1)=O.Cl.[CH3:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][NH2:25])=[CH:20][CH:19]=1.C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH3:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[CH:1]=[C:3]([C:4]3[N:9]=[C:8]([C:10]([OH:12])=[O:11])[CH:7]=[CH:6][CH:5]=3)[CH:13]=[N:25]2)=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 27239044-Methoxyphenylhydrazine hydrochlorideHCID 27352046-(1,3-Dioxopropan-2-yl)picolinic acid

생성물 1

HCID 11630741HCID 11630741, 화합물수율 61%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 6-(diformylmethyl)-pyridin-2-carboxylic acid (315 mg, 1.63 mmol), 4-methoxyphenylhydrazine hydrochloride (285 mg, 1.63 mmol) and sodium acetate (134 mg, 1.63 mmol) in acetic acid (5 mL) is heated to 110° C. for 18 h. After being allowed to cool, the solution is filtered. The solid product is washed with ethyl acetate and diethyl ether, and dried under vacuum to afford the title product (294 mg, 0.99 mmol, 61%) as a beige powder. m.p. 122-123° C. 1H NMR (300 MHz, DMSO-d6): δ 9.11 (1H, s), 8.38 (1H, s), 7.99 (2H, d, J=4.7 Hz), 7.86 (1H, t, J=4.4 Hz), 7.80 (2H, d, J=9.1 Hz), 7.08 (2H, d, J=9.1 Hz), 3.80 (3H, s), 1H missing. MS (ES+): m/e 297 (18), 296 (100). MS (ES−): m/e 295 (14), 294 (100).

후처리

  1. temperatureto cool
  2. filtrationthe solution is filtered
  3. washThe solid product is washed with ethyl acetate and diethyl ether
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-ead393ce1a5147838c4fe00b3a13a71c
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051342B2

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