Sodium sulfate decahydrate → N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide

HRID 1432074

반응식

HRID 1432074 반응식
[C:1]([NH:4][C:5]1[C:12]([Cl:13])=[CH:11][C:8]([C:9]#[N:10])=[CH:7][C:6]=1[Cl:14])(=[O:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[C:1]([NH:4][C:5]1[C:6]([Cl:14])=[CH:7][C:8]([CH2:9][NH2:10])=[CH:11][C:12]=1[Cl:13])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 2735977N-(2,6-dichloro-4-cyanophenyl)acetamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 58962993N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide수율 30%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Step AT2. To a solution of 4-acetamido-3,5-dichloro-benzonitrile (114 mg, 0.5 mmol) in 5 mL of THF was added lithium aluminum hydride (120 mg, 3.2 mmol) in portion and the resulting mixture was stirred for 3 hours. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in portion and the mixture was stirred for 30 minutes. The solid was filtered off and the filtration was concentrated. Residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%).

후처리

  1. stirringthe mixture was stirred for 30 minutes
  2. filtrationThe solid was filtered off
  3. filtrationthe filtration
  4. concentrationwas concentrated
  5. customResidue was purified by HPLC

출처 및 근거

ORD 기록
ord-27e4930584df49deaf113f207d70c4b4
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612069B2

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