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

HRID 133785

반응식

HRID 133785 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 B (2): 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 one portion and the resulting mixture was stirred for 3 h. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in one portion and the mixture was stirred for 30 min. The solid was filtered off and the filtrate was concentrated. The residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%). 1H NMR (500 MHz, CD3OD): δ 7.46 (s, 2 H), 3.78 (s, 2H), 2.18 (s, 3 H).

후처리

  1. stirringthe mixture was stirred for 30 min
  2. filtrationThe solid was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-cc504b15272a48c7a93affceaa977dc8
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390925B2

연결된 노트

불러오는 중…