Triethylamine → METHYL 3-(HYDROXYMETHYL)-5-NITROBENZOATE

HRID 1531939

反応式

HRID 1531939 の反応式
Cl[C:2]([C:4]1[CH:5]=[C:6]([CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=1)[C:7]([O:9][CH3:10])=[O:8])=[O:3].[BH4-].[Na+].C(N(CC)CC)C>O1CCOCC1>[OH:3][CH2:2][C:4]1[CH:5]=[C:6]([CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=1)[C:7]([O:9][CH3:10])=[O:8]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 74774Methyl 3-(chlorocarbonyl)-5-nitrobenzoateHCID 4311764Sodium borohydride

生成物 1

HCID 10703703METHYL 3-(HYDROXYMETHYL)-5-NITROBENZOATE

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A stirred solution of the product from step (i) (46.54 g) and sodium borohydride (13.01 g) in 1,4-dioxane (200 ml) was heated at reflux for 17 hours. The mixture was cooled and treated with triethylamine (27.9 ml), poured onto ice-water and extracted with ethyl acetate. The combined extracts were dried (MgSO4) and evaporated. The product was recrystallised from isohexane. Yield 19.38 g.

後処理

  1. temperatureat reflux for 17 hours
  2. temperatureThe mixture was cooled
  3. additionpoured onto ice-water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. customevaporated
  7. customThe product was recrystallised from isohexane

出典と根拠

ORDレコード
ord-8ae2dc45fa73405cbbda1d2570d69ebf
出典データセット
uspto-grants-2001_03
特許番号
US06200981B1

関連ノート

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