Ethoxyethylamine → N-(2-ethoxyethyl)-3-fluoro-4-nitrobenzamide

HRID 72766

반응식

HRID 72766 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5]([OH:7])=O.[CH2:14]([O:16][CH2:17][CH2:18][NH2:19])[CH3:15].C(N(CC)C(C)C)(C)C.Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1>Cl.C(#N)C>[CH2:14]([O:16][CH2:17][CH2:18][NH:19][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([N+:11]([O-:13])=[O:12])=[C:2]([F:1])[CH:3]=1)[CH3:15]

참가 물질

8

반응물 5

HCID 66970EthoxyethylamineHCID 81531DiisopropylethylamineHCID 2306533-Fluoro-4-nitrobenzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrate

생성물 1

HCID 59198706N-(2-ethoxyethyl)-3-fluoro-4-nitrobenzamide

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 6342Acetonitrile용매

실험 절차

3-Fluoro-4-nitrobenzoic acid 5.55 g, 2-ethoxyethylamine 3.15 mL, N,N-diisopropylethylamine 5.23 mL, 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride 8.63 g, 1-hydroxybenzotriazole monohydrate 5.96 g and acetonitrile 77 mL were mixed and stirred for 19 hours. The reaction liquid was poured in diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with saturated brine, saturated aqueous sodium hydrogencarbonate solution and saturated brine, by the order stated, and dried over magnesium sulfate. Distilling the solvent off, 6.86 g of the title compound was obtained.

후처리

  1. customThe reaction liquid
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated brine, saturated aqueous sodium hydrogencarbonate solution and saturated brine, by the order
  4. dry with materialdried over magnesium sulfate
  5. distillationDistilling the solvent off, 6.86 g of the title compound
  6. customwas obtained

출처 및 근거

ORD 기록
ord-c289596415db46dba95edc6d7a6a7ad7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829000B2

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