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

HRID 14401

반응식

HRID 14401 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 hours. Then, sodium sulfate decahydrate (4.83 g, 15 mmol) was added and stirred for 30 min. The solid was filtered off and washed with THF for three times. The solvent was removed by rotovap and residue was purified by column 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): δ 7.2 (s, 2H), 3.65 (s, 2H).

후처리

  1. stirringstirred for 30 min
  2. filtrationThe solid was filtered off
  3. washwashed with THF for three times
  4. customThe solvent was removed by rotovap and residue
  5. customwas purified by column with Methanol/DCM (3:7) as the eluant

출처 및 근거

ORD 기록
ord-ed8d7956d0384a1687ead6d120fd7703
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732434B2

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