Sodium borohydride → 3,5-dichloro-4-hydroxymethyl-N-methylaniline

HRID 1290167ノート

反応式

HRID 1290167 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:12])[C:9]=1[CH:10]=[O:11])[NH:5][CH3:6].[BH4-].[Na+]>CO.O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:12])[C:9]=1[CH2:10][OH:11])[NH:5][CH3:6]

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 18923365HCID 18923365、化合物

生成物 1

HCID 189235483,5-dichloro-4-hydroxymethyl-N-methylaniline収率 100.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3,5-dichloro-4-formyl-N-methylaniline (242 mg) in methanol (3 ml) and tetrahydrofuran (3 ml) was added sodium borohydride (45 mg) and the mixture was stirred for 30 minutes at ambient temperature. The reaction mixture was quenched with aqueous saturated ammonium chloride solution and ethyl acetate was added thereto. The separated organic layer was washed with aqueous saturated ammonium chloride solution, dried and concentrated in vacuo to give 3,5-dichloro-4-hydroxymethyl-N-methylaniline (246 mg).

後処理

  1. customThe reaction mixture was quenched with aqueous saturated ammonium chloride solution and ethyl acetate
  2. additionwas added
  3. washThe separated organic layer was washed with aqueous saturated ammonium chloride solution
  4. customdried
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-af329abe7e2f445ba79cfc209a513b35
出典データセット
uspto-grants-1998_05
特許番号
US05750699

反応ノート

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