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Methylamine → HCID 18176647, 화합물

HRID 394485
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HRID 394485 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[C:9]([Cl:14])[CH:8]=1.[CH3:15][NH2:16].[O-2].[Ca+2]>C1COCC1>[Cl:14][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][C:10]=1[Cl:13])[O:6][CH2:5][CH2:4][CH2:3][CH2:2][NH:16][CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 6850728CalciumoxideHCID 187686344-(4-Bromobutoxy)-1,2-dichlorobenzene

생성물 1

HCID 18176647HCID 18176647, 화합물수율 80.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
125 °C

실험 절차

A mixture of 4-(4-bromobutoxy)- 1,2-dichlorobenzene (0.03 mol), methylamine (20 g) and calciumoxide (7 g) in THF (100 ml) was stirred at 125° C. overnight in an autoclave. The mixture was filtered over dicalite and the filtrate was evaporated. The residue was taken up in DIPE and the mixture was filtered over dicalite. The filtrate was converted into the hydrochloric acid salt (1:1) with HCl/2-propanol. The precipitate was filtered off and dried, yielding 6 g (70.3%) of 4-(3,4-dichlorophenoxy)-N-methyl-1-butanamine (intermediate 4, mp. 132° C.).

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. filtrationThe mixture was filtered over dicalite
  2. customthe filtrate was evaporated
  3. filtrationthe mixture was filtered over dicalite
  4. filtrationThe precipitate was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-7d09998466384c6996cf8fb9602ffc90
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06602873B2

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