1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 21997505, 화합물

HRID 1977300노트

반응식

HRID 1977300 반응식
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][CH:7]=1)=[O:5].[CH2:13]([O:20][C:21]1[CH:29]=[CH:28][C:24]([C:25](O)=[O:26])=[CH:23][CH:22]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].ON1C2C=CC=CC=2N=N1.C(N=C=NCCCN(C)C)C>ClCCl>[CH2:13]([O:20][C:21]1[CH:22]=[CH:23][C:24]([C:25]([NH:2][CH2:3][C:4]([C:6]2[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][CH:7]=2)=[O:5])=[O:26])=[CH:28][CH:29]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]

참가 물질

6

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 85154p-Heptoxybenzoic acidHCID 27982162-Amino-1-(4-bromophenyl)ethan-1-one hydrochloride

생성물 1

HCID 21997505HCID 21997505, 화합물수율 78%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-amino-4′-bromoacetophenone hydrochloride (5.0 g), 4-heptyloxybenzoic acid (4.72 g) and 1-hydroxybenzotriazole (2.7 g) in dichloromethane (50 ml) was added 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide (WSCD) (3.65 ml) and the mixture was stirred for 3 hours at ambient temperature. The reaction mixture was diluted with dichloromethane (200 ml), and washed with water, 1N hydrochloric acid, saturated sodium hydrogen carbonate aqueous solution and brine. The organic layer was dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The solids were slurried in ethyl acetate and collected by filtration to give 2-(4-heptyloxybenzoylamino)-4′-bromoacetophenone (6.73 g).

후처리

  1. washwashed with water, 1N hydrochloric acid, saturated sodium hydrogen carbonate aqueous solution and brine
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationMagnesium sulfate was filtered off
  4. customthe filtrate was evaporated under reduced pressure
  5. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-01cda527458345b098604eb199b7d2fd
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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