Lithium hydroxide, monohydrate → 2-(2-Thiazolinylthio)-hydrocinnamic acid

HRID 478042ノート

反応式

HRID 478042 の反応式
C([O:3][C:4](=[O:19])[CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[S:13][C:14]1[S:15][CH2:16][CH2:17][N:18]=1)C.O.[OH-].[Li+]>C1COCC1.O>[S:15]1[CH2:16][CH2:17][N:18]=[C:14]1[S:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[CH2:6][CH2:5][C:4]([OH:19])=[O:3]

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 572061812-(2-Thiazolinylthio)hydrocinnamic acid ethyl ester

生成物 1

HCID 570633422-(2-Thiazolinylthio)-hydrocinnamic acid

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

A mixture of 250 mg of 2-(2-thiazolinylthio)hydrocinnamic acid ethyl ester, 36 mg of lithium hydroxide monohydrate and 5 ml of THF/water 9:1 is stirred at room temperature for 5 days and then concentrated to dryness by evaporation. The residue is taken up in water, washed with ethyl acetate, adjusted to pH 5 with 0.5N HCl and extracted with ethyl acetate. The extracts are washed with water, dried with sodium sulphate, concentrated by evaporation and chromatographed on silica gel with eluant R. Rf (R)=0.22.

後処理

  1. concentrationconcentrated to dryness by evaporation
  2. washwashed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. washThe extracts are washed with water
  5. dry with materialdried with sodium sulphate
  6. concentrationconcentrated by evaporation
  7. customchromatographed on silica gel with eluant R

出典と根拠

ORDレコード
ord-3f39a6c491db44bc861b222258d43e47
出典データセット
uspto-grants-1989_12
特許番号
US04889869

反応ノート

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