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Hydrochloric Acid → (2-Chloro-4-fluoro-5-nitrophenyl)methanol

HRID 231429
ノート
印刷プレビュー

反応式

HRID 231429 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]=1[CH:4]=[O:5].[BH4-].[Na+].Cl>O1CCCC1>[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]=1[CH2:4][OH:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 135637752-Chloro-4-fluoro-5-nitrobenzaldehyde

生成物 1

HCID 13629752(2-Chloro-4-fluoro-5-nitrophenyl)methanol収率 70.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 10.8 g (0.053 mole) of 2-chloro-4-fluoro-5-nitrobenzaldehyde in 100 ml of tetrahydrofuran was added 0.50 g (0.013 mole) of sodium borohydride portionwise. The reaction mixture was stirred for one hour after which dilute hydrochloric acid was added to destroy unreacted sodium borohydride. To this mixture was added 200 ml of methylene chloride, and the phases were separated. The organic phase was washed three times with water, dried over anhydrous magnesium sulfate, and filtered. The solvent was evaporated from the filtrate under reduced pressure, leaving a residue weighing 10.7 g. This residue was combined with 1.67 g of a similar residue another run of the same reaction. The combined residues were passed through a silica gel column, eluting with ethyl acetate/heptane (1/4) to yield 7.7 g of 2-chloro-4-fluoro-5-nitrobenzyl alcohol as a yellow solid.

後処理

  1. additionwas added
  2. customto destroy unreacted sodium borohydride
  3. additionTo this mixture was added 200 ml of methylene chloride
  4. customthe phases were separated
  5. washThe organic phase was washed three times with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customThe solvent was evaporated from the filtrate under reduced pressure
  9. customleaving a residue
  10. customanother run of the same reaction
  11. washeluting with ethyl acetate/heptane (1/4)

出典と根拠

ORDレコード
ord-ef30e54f9f504dd79a79c8a1ed3a5323
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04846882

反応ノート

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