Hydrochloric Acid → 92188-54-0

HRID 1638735ノート

反応式

HRID 1638735 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10](=[N:12][OH:13])[CH3:11])=[CH:5][CH:4]=1.[ClH:14].[BH3-]C#N.[Na+]>CO>[ClH:14].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH:10]([NH:12][OH:13])[CH3:11])=[CH:5][CH:4]=1

参加物

5

実験手順

23.7 g (0.13 mol) of 4-methoxyphenylacetone oxime were dissolved in 200 ml of methanol and the solution was brought to pH 3 with dilute hydrochloric acid. 8.3 g (0.13 mol) of NaBH3CN were then introduced in portions, the pH being kept at 3 by simultaneous addition of dilute hydrochloric acid. The mixture was subsequently stirred overnight at room temperature, the pH was brought to 1 with hydrochloric acid and the mixture was evaporated. The aqueous residue was extracted with methylene chloride (3×100 ml). The combined organic phases were washed with water (3×25 ml), dried over Na2SO4 and evaporated. Yield 23.3 g (80% of theory), melting point 124° C.

後処理

  1. customthe mixture was evaporated
  2. extractionThe aqueous residue was extracted with methylene chloride (3×100 ml)
  3. washThe combined organic phases were washed with water (3×25 ml)
  4. dry with materialdried over Na2SO4
  5. customevaporated

出典と根拠

ORDレコード
ord-01dadd4a844949f7a5559bddf1e9956e
出典データセット
uspto-grants-1989_11
特許番号
US04880840

反応ノート

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