4-Chlorobenzoyl chloride → 4-Chloro-N-[[2-[2-(4-morpholinyl)ethoxy]phenyl]methyl]-N-(2-phenylethyl)benzamide, hydrochloride salt

HRID 26968

반응식

HRID 26968 반응식
[N:1]1([CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH2:16][NH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31](Cl)=[O:32])=[CH:29][CH:28]=1>C(Cl)(Cl)Cl.CCOCC>[ClH:26].[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31]([N:17]([CH2:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH2:8][CH2:7][N:1]2[CH2:2][CH2:3][O:4][CH2:5][CH2:6]2)[CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:32])=[CH:29][CH:28]=1

참가 물질

5

반응물 2

HCID 85014-Chlorobenzoyl chlorideHCID 21322749N-[[2-[2-(4-Morpholinyl)ethoxy]phenyl]methyl]benzeneethanamine

생성물 1

HCID 1317113154-Chloro-N-[[2-[2-(4-morpholinyl)ethoxy]phenyl]methyl]-N-(2-phenylethyl)benzamide, hydrochloride salt수율 168.8%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6212Chloroform용매

실험 절차

N-[[2-[2-(4-Morpholinyl)ethoxy]phenyl]methyl]benzeneethanamine (40 g) and 22 g of p-chlorobenzoyl chloride are reacted in 600 ml of chloroform following the procedure described in Example 1C. The residue from the chloroform evaporation is first triturated with ether (evaporation repeated) and then with 400 ml of warm acetone to give a crystalline product. After diluting with 500 ml of ether and cooling for about 16 hours, the solid is filtered under nitrogen, washed with ether and dried in vacuo to yield 54.7 g of material, melting point 147°-149° C. (sintering at 145° C.). Crystallization from 250 ml of warm methanol-1750 ml ether yield 52.9 g of the title compound, melting point 147°-149° C.

후처리

  1. customThe residue from the chloroform evaporation
  2. customis first triturated with ether (evaporation repeated)
  3. customwith 400 ml of warm acetone to give a crystalline product
  4. temperaturecooling for about 16 hours
  5. filtrationthe solid is filtered under nitrogen
  6. washwashed with ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-ef7f1125e2584476ae7a2f558029ebd1
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151354

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