Toluene → (2,3-Dichloro-6-nitrophenyl)methanol

HRID 41351

反応式

HRID 41351 の反応式
C1(C)C=CC=CC=1.[Cl:8][C:9]1[C:16]([Cl:17])=[CH:15][CH:14]=[C:13]([N+:18]([O-:20])=[O:19])[C:10]=1[CH:11]=[O:12].[BH4-].[Na+]>CO>[Cl:8][C:9]1[C:16]([Cl:17])=[CH:15][CH:14]=[C:13]([N+:18]([O-:20])=[O:19])[C:10]=1[CH2:11][OH:12]

参加物

5

反応物 3

HCID 1140TolueneHCID 4311764Sodium borohydrideHCID 112182712,3-Dichloro-6-nitrobenzaldehyde

生成物 1

HCID 11160370(2,3-Dichloro-6-nitrophenyl)methanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

To form 2,3-dichloro-6-nitrobenzylalcohol (compound XX) from 2,3-dichloro-6-nitro benzaldehyde (compound XIX), compound XIX is preferably solubilized in a solvent or solvent mixture such as toluene and methanol. The solution of compound XIX is added to a reducing solution such as sodium borohydride in an organic solvent over a period of time to maintain a reaction temperature below about 40° C., preferably 25° C. The reaction is preferably stirred for 24 hours at room temperature under nitrogen and then washed with water. After removing the aqueous layer the organic layer is azeotropically dried and concentrated forming 2,3-dichloro-6-nitrobenzylalcohol (compound XX).

後処理

  1. washwashed with water
  2. customAfter removing the aqueous layer the organic layer
  3. customis azeotropically dried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4b7498d6d4404f80b161caa37cf7fac8
出典データセット
uspto-grants-2013_09
特許番号
US08530651B2

関連ノート

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