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Benzenemethanamine, 3,4-dichloro- → HCID 59474755, 화합물

HRID 1966509
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HRID 1966509 반응식
[CH3:1][N:2]([CH3:18])[S:3]([C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[C:11]2Cl)(=[O:5])=[O:4].[Cl:19][C:20]1[CH:21]=[C:22]([CH:25]=[CH:26][C:27]=1[Cl:28])[CH2:23][NH2:24]>CO>[CH3:1][N:2]([CH3:18])[S:3]([C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[C:11]2[NH:24][CH2:23][C:22]1[CH:25]=[CH:26][C:27]([Cl:28])=[C:20]([Cl:19])[CH:21]=1)(=[O:5])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1608Benzenemethanamine, 3,4-dichloro-HCID 59474736HCID 59474736, 화합물

생성물 1

HCID 59474755HCID 59474755, 화합물수율 13%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-Chloro-2-methylquinoline-8-sulfonic dimethylamide (80 mg, 0.281 mmole) and 3,4-dichlorobenzylamine (100 mg, 0.568 mmole) were stirred at 155° C. for 10 min in a microwave oven. Methanol was added and the mixture was concentrated, mixed with dichloromethane and then filtered. The residue was purified using silica gel chromatography, eluting with dichloromethane:methanol 95:5. Precipitation in ethyl acetate gave a pink solid (15 mg, 13%).

후처리

  1. concentrationthe mixture was concentrated
  2. additionmixed with dichloromethane
  3. filtrationfiltered
  4. customThe residue was purified
  5. washeluting with dichloromethane:methanol 95:5
  6. customPrecipitation in ethyl acetate

출처 및 근거

ORD 기록
ord-a0e3960596a34de0a31b3fece07f5b39
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420670B2

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