Water → 2',5-Dichloro-2-methylaminobenzhydrol

HRID 617093ノート

反応式

HRID 617093 の反応式
[BH4-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[O:20])[C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[NH:18][CH3:19].O>O1CCCC1>[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([OH:20])[C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[NH:18][CH3:19]

参加物

5

反応物 3

HCID 962Water2 回HCID 21833Benzophenone, 2',5-dichloro-2-methylamino-HCID 4311764Sodium borohydride

生成物 1

HCID 124217352',5-Dichloro-2-methylaminobenzhydrol収率 97.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of sodium borohydride (1.2 g) in tetrahydrofuran (10 ml), a solution of 2',5-dichloro-2-methylaminobenzophenone (3.12 g) in tetrahydrofuran (20 ml) is added dropwise. The resultant mixture is mixed with water (5 ml) and stirred at room temperature overnight. The reaction mixture is mixed with a small amount of water and evaporated under reduced pressure to remove the solvent. The residue is made to pH 8-9 with dilute hydrochloric acid and shaken with chloroform. The organic layer is dried and evaporated to give 2', 5-dichloro-2-methylaminobenzhydrol (3.05 g). This substance is recrystallized from ether/n-hexane to give crystals melting at 105.5° to 106.5° C. The yield is 97.1%.

後処理

  1. customevaporated under reduced pressure
  2. customto remove the solvent
  3. stirringshaken with chloroform
  4. customThe organic layer is dried
  5. customevaporated

出典と根拠

ORDレコード
ord-5609b3e1d27043ecbfb1870dd79cdb9f
出典データセット
uspto-grants-1978_02
特許番号
US04076702

反応ノート

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