Methanol → HCID 20388954、化合物

HRID 437942ノート

反応式

HRID 437942 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 20388954HCID 20388954、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7241114827ce4efd856d323484e2efc5
出典データセット
uspto-grants-1977_06
特許番号
US04032643

反応ノート

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