Chloroacetic Acid → HCID 18779028、化合物

HRID 1741445ノート

反応式

HRID 1741445 の反応式
[H-].[Na+].[CH3:3][C:4]1[S:8][C:7]([CH2:9][CH2:10][OH:11])=[CH:6][CH:5]=1.Cl[CH2:13][C:14]([OH:16])=[O:15]>CN(C)C=O>[CH3:3][C:4]1[S:8][C:7]([CH2:9][CH2:10][O:11][CH2:13][C:14]([OH:16])=[O:15])=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 300Chloroacetic AcidHCID 24758Sodium hydrideHCID 1328928919498-70-5

生成物 1

HCID 18779028HCID 18779028、化合物収率 107.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

Sodium hydride (0.622 g) was suspended in dry dimethylformamide (5 ml) and treated dropwise with a solution of 2-(5-methyl-2-thienyl)ethanol (1.0 g) in dry dimethylformamide (5 ml). The mixture was stirred at room temperature under nitrogen for 2 hours then a solution of chloroacetic acid (0.664 g) in dry dimethylformamide (5 ml) added. The mixture was stirred at room temperature overnight. The volatiles were removed in vacuo and the residue quenched with water and extracted with ethyl acetate. The aqueous layer was adjusted to pH 2 using dilute hydrochloric acid and then extracted with ethyl acetate. This extract was washed with water, brine then dried (MgSO4). The solvent was removed in vacuo to give a brown oil (1.51 g) which was used without further purification.

後処理

  1. stirringThe mixture was stirred at room temperature overnight
  2. customThe volatiles were removed in vacuo
  3. customthe residue quenched with water
  4. extractionextracted with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. washThis extract was washed with water, brine
  7. dry with materialthen dried (MgSO4)
  8. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-a38cabd90e2542f69709927a39361529
出典データセット
uspto-grants-1999_10
特許番号
US05973167

反応ノート

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