Triethylamine → HCID 22112924, 화합물

HRID 726305노트

반응식

HRID 726305 반응식
[NH2:1][CH2:2][C:3]([N:5]([C:7]1[C:8]([Cl:27])=[C:9]([C:23]([Cl:26])=[CH:24][CH:25]=1)[CH2:10][O:11][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]2[C:21]=1[N:20]=[C:19]([CH3:22])[CH:18]=[CH:17]2)[CH3:6])=[O:4].C(N(CC)CC)C.Br[CH2:36][C:37](Cl)=[O:38].[CH3:40][NH:41][CH:42]1[CH2:48][CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]1>ClCCl>[CH:42]1([N:41]([CH3:40])[CH2:36][C:37]([NH:1][CH2:2][C:3]([N:5]([C:7]2[C:8]([Cl:27])=[C:9]([C:23]([Cl:26])=[CH:24][CH:25]=2)[CH2:10][O:11][C:12]2[CH:13]=[CH:14][CH:15]=[C:16]3[C:21]=2[N:20]=[C:19]([CH3:22])[CH:18]=[CH:17]3)[CH3:6])=[O:4])=[O:38])[CH2:48][CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 89602Bromoacetyl chlorideHCID 276275N-cycloheptyl-N-methylamineHCID 117954848-[3-(N-glycyl-N-methylamino)2,6-dichlorobenzyloxy]-2-methylquinoline

생성물 1

HCID 22112924HCID 22112924, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 8-[3-(N-glycyl-N-methylamino)-2,6-dichlorobenzyloxy]-2-methylquinoline (150 ml), triethylamine (0.077 ml) and dichloromethane (1.5 ml) was added bromoacetyl chloride (0.034 ml) in a dry ice-acetone bath. After 30 minutes, to the mixture was added N-methyl-N-cycloheptylamine (236 mg). The mixture was stirred for 3 hours at ambient temperature. The reaction mixture was washed with aqueous sodium bicarbonate solution, water and brine. The organic layer was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a silica gel column chromatography (dichloromethane-methanol) to yield 8-[3-[N-[(N-cycloheptyl-N-methylglycyl)glycyl]-N-methylamino]-2,6-dichlorobenzyloxy]-2-methylquinoline (151 mg) as amorphous.

후처리

  1. washThe reaction mixture was washed with aqueous sodium bicarbonate solution, water and brine
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. customevaporated in vacuo
  4. customThe residue was purified by a silica gel column chromatography (dichloromethane-methanol)

출처 및 근거

ORD 기록
ord-e05f47152bb24722be7ccfae9bc214f9
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05708173

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