Glyoxylic acid, monohydrate → Hwa 131

HRID 1165133노트

반응식

HRID 1165133 반응식
O.[C:2]([OH:6])(=O)[CH:3]=O.Br.[NH2:8][C:9]1[S:10][CH2:11][C:12]([C:15]2[CH:20]=[C:19]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:18]([OH:25])=[C:17]([C:26]([CH3:29])([CH3:28])[CH3:27])[CH:16]=2)=[N:13][N:14]=1>O.C(O)(=O)C.Cl>[C:26]([C:17]1[CH:16]=[C:15]([C:12]2[N:14]3[N:13]=[CH:3][C:2](=[O:6])[N:8]=[C:9]3[S:10][CH:11]=2)[CH:20]=[C:19]([C:21]([CH3:24])([CH3:22])[CH3:23])[C:18]=1[OH:25])([CH3:29])([CH3:27])[CH3:28]

참가 물질

6

반응물 2

HCID 15620607Glyoxylic acid, monohydrateHCID 136364585HCID 136364585, 화합물

생성물 1

HCID 159492Hwa 131

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

4.8 g (0.05 mol) of glyoxylic acid monohydrate in 75 ml of water were added dropwise to a solution of 10.0 g (0.025 mol) of 2-amino-5-(3,5-di-tert.butyl-4-hydroxyphenyl)-6H-1,3,4-thiadiazine hydrobromide from step (c1) in 250 ml of glacial acetic acid and 25 ml of 4N hydrochloric acid at 80° C. After the mixture had been stirred at 80° C. for 20 hours, it was evaporated under reduced pressure. It was advantageously possible to purify the solid residue by column chromatography on silica gel using methylene chloride/methanol (25:1) as the eluent and subsequent recrystallization from ethanol, and, from analytical and spectroscopic investigations, the product proved to be identical to that prepared by procedures (a) and (b).

후처리

  1. customit was evaporated under reduced pressure
  2. customto purify the solid residue by column chromatography on silica gel
  3. customas the eluent and subsequent recrystallization from ethanol
  4. customthat prepared by procedures (a) and (b)

출처 및 근거

ORD 기록
ord-bddf200e56554c92af1d877521486423
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04908364

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