Methanol → HCID 20388954、化合物

HRID 616378ノート

反応式

HRID 616378 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-thiazole-propanoic acid, 3.2 ml of concentrated sulfuric acid and 300 ml of methanol was refluxed for 16 hours and was concentrated under reduced pressure. The mixture was added to 100 ml of water and concentrated ammonium hydroxide was added to obtain a pH of 12-13. The mixture was extracted with methylene chloride and the organic extracts were dried over magnesium sulfate and concentrated to dryness under reduced pressure to obtain 35 g of raw methyl 2-methyl-5-thiazole-propanoate. The hydrochloride thereof melted at 115° C.

後処理

  1. temperaturewas refluxed for 16 hours
  2. concentrationwas concentrated under reduced pressure
  3. additionThe mixture was added to 100 ml of water and concentrated ammonium hydroxide
  4. additionwas added
  5. customto obtain a pH of 12-13
  6. extractionThe mixture was extracted with methylene chloride
  7. dry with materialthe organic extracts were dried over magnesium sulfate
  8. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-fa6f02bdf00c4453af5a2a0b63fa4a4a
出典データセット
uspto-grants-1978_02
特許番号
US04073919

反応ノート

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