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

HRID 133783

반응식

HRID 133783 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 189757634-Amino-3,5-dichlorobenzylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-23b29a36e2744324a60f1f48f7bb42a5
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390925B2

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