Hydrochloric Acid → 2-(2,3-Difluoro-4-(2-hydroxyethyl)phenoxy)acetaldehyde

HRID 471169ノート

反応式

HRID 471169 の反応式
Cl.C([O:4][CH:5](OCC)[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][OH:16])=[C:10]([F:17])[C:9]=1[F:18])C>O1CCOCC1.O>[F:18][C:9]1[C:10]([F:17])=[C:11]([CH2:14][CH2:15][OH:16])[CH:12]=[CH:13][C:8]=1[O:7][CH2:6][CH:5]=[O:4]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 579889892-(4-(2,2-Diethoxyethoxy)-2,3-difluorophenyl)ethanol

生成物 1

HCID 866367532-(2,3-Difluoro-4-(2-hydroxyethyl)phenoxy)acetaldehyde

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

Concentrated hydrochloric acid (5 mL) was added to a solution of 2-(4-(2,2-diethoxyethoxy)-2,3-difluorophenyl)ethanol (example 77, step c) (0.49 g) in 1,4-dioxane (10 mL) and the resulting mixture was stirred for 1 h. The mixture was carefully diluted with water (50 mL) and extracted with ethyl acetate (3×50 mL). The combined organics were washed with water (50 mL) and brine (50 mL), dried over sodium sulphate, filtered and evaporated to give the subtitled compound, which was used directly. Yield 0.31 g.

後処理

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. washThe combined organics were washed with water (50 mL) and brine (50 mL)
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-d9371c8a2384405bb422374284e2c1fb
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

反応ノート

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