Methanol → HCID 20388954, 화합물

HRID 437942노트

반응식

HRID 437942 반응식
[CH3:1][C:2]1[S:3][C:4]([CH2:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:5][N:6]=1.S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[S:3][C:4]([CH2:7][CH2:8][C:9]([O:11][CH3:17])=[O:10])=[CH:5][N:6]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 203889533-(2-methyl-1,3-thiazol-5-yl)propanoic acid

생성물 1

HCID 20388954HCID 20388954, 화합물

실험 절차

A mixture of 31.7 g of 2-methyl-5-thiazolepropanoic acid, 3.2 ml of concentrated sulfuric acid and 300 ml of methanol was refluxed for 16 hours and was then concentrated to dryness. The residue was taken up in 100 ml of water and the pH was adjusted to 12-13 with addition of concentrated ammonium hydroxide. The mixture was extracted with methylene chloride and the extracts were dried over magnesium sulfate and was evaporated to dryness under reduced pressure to obtain 35 g of raw methyl 2-methyl-5-thiazolepropanoate. Its hydrochloride had a melting point of 115° C.

후처리

  1. temperaturewas refluxed for 16 hours
  2. concentrationwas then concentrated to dryness
  3. additionthe pH was adjusted to 12-13 with addition of concentrated ammonium hydroxide
  4. extractionThe mixture was extracted with methylene chloride
  5. dry with materialthe extracts were dried over magnesium sulfate
  6. customwas evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-7241114827ce4efd856d323484e2efc5
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032643

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