1,2-Dichloroethane → HCID 22326844, 화합물

HRID 491619노트

반응식

HRID 491619 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, H2O 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, H2O and brine
  2. customRemoval of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-12afe95e839b42e0a1b45d0d17319974
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531553B2

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