Sodium sulfate decahydrate → 4-Amino-3,5-dichlorobenzylamine

HRID 133783

反応式

HRID 133783 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([Cl:17])[C:15]=1[NH2:16])[C:11]#[N:12].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[Cl:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([Cl:17])[C:15]=1[NH2:16])[CH2:11][NH2:12]

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 5227064-Amino-3,5-dichlorobenzonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 189757634-Amino-3,5-dichlorobenzylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To lithium aluminum hydride (0.57 g, 15 mmol) in dry THF (20 mL) was added dropwise 3,5-dichloro-4-aminobenzonitrile (1.87 g, 10 mmol) in THF (30 mL). The mixture was stirred at rt for 2 h. Then, sodium sulfate decahydrate (4.83 g, 15 mmol) was added and the mixture was stirred for 30 min. The solid was filtered off and washed with THF three times. The solvent was removed under vacuum and the residue was purified by chromatography with Methanol/DCM (3:7) as the eluant. 3,5-Dichloro-4-aminobenzylamine was obtained as an off-white solid (1.5 g, 80%). 1H NMR (300 MHz, CD3OD): δ3.65 (s, 2H), 7.2 (s, 2H).

後処理

  1. stirringthe mixture was stirred for 30 min
  2. filtrationThe solid was filtered off
  3. washwashed with THF three times
  4. customThe solvent was removed under vacuum
  5. customthe residue was purified by chromatography with Methanol/DCM (3:7) as the eluant

出典と根拠

ORDレコード
ord-23b29a36e2744324a60f1f48f7bb42a5
出典データセット
uspto-grants-2008_06
特許番号
US07390925B2

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