1,2-Dichloroethane → HCID 22326844, 화합물

HRID 495455노트

반응식

HRID 495455 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:4]=1[CH2:12][C:13]([OH:15])=O.C(Cl)CCl.C[CH2:21][N:22](CC)[CH2:23]C.Cl.CNC>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:4]=1[CH2:12][C:13]([N:22]([CH3:23])[CH3:21])=[O:15]

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 35192982-(2-methoxy-5-nitrophenyl)acetic acid

생성물 1

HCID 22326844HCID 22326844, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-(2-Methoxy-5-nitrophenyl)acetic acid (17.1 g, 1 eq, Step B), EDC (18.6 g, 1.2 eq.), Et3N (9.8 g, 13.6 mL, 1.2 eq) and dimethylamine hydrochloride (7.9 g, 1.2 eq.) in 150 mL of CH2Cl2 were stirred together with exclusion of air overnight. CH2Cl2 (150 mL) was added and the mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine. Removal of the solvent under reduced pressure followed by silica gel chromatography (90:10 CH2Cl2:EtOAc) afforded pure 2-(2-methoxy-5-nitrophenyl)-N,N-dimethyl-acetamide as a white solid.

후처리

  1. washthe mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine
  2. customRemoval of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-a6595046bb5b4d8dbbd4426b89f2d4ff
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939874B2

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