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Water → HCID 14151565, 화합물

HRID 2165998
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HRID 2165998 반응식
[C:1]([CH2:9][C:10]([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:19]([NH2:23])[CH2:20][CH2:21][CH3:22].O.C(C1(C)[O:32][C:31](=O)[CH:30]=[C:29]([CH3:34])O1)C>C(O)(=O)C.C1(C)C=CC=CC=1>[CH2:19]([N:23]1[C:29]([CH3:34])=[CH:30][C:31](=[O:32])[C:9]([C:10]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:11])=[C:1]1[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH2:20][CH2:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8007Butylamine2회HCID 703983-Oxo-3-phenylpropionanilideHCID 10534915HCID 10534915, 화합물

생성물 1

HCID 14151565HCID 14151565, 화합물수율 55.9%

시약·촉매·용매 2

HCID 176Acetic Acid촉매
HCID 1140
Toluene
용매
2회

실험 절차

A mixture of 4.42 g (18.47 mmol) of α-benzoylacetanilide, 1.89 g (25.84 mmol) of n-butylamine, one drop of acetic acid and 25 ml of toluene was refluxed for 1.5 hours, while the resulted water and excess of butylamine were removed through a Dean-Stark's water separator, together with about 12 ml of toluene. While heating, to the mixture was dropwise added a solution of 7.2 g (46.18 mmol) of 2-ethyl-2,6-dimethyl-4H-1,3-dioxin-4-one in 16 ml of toluene within about 30 minutes and after the resulted mixture was refluxed for forty minutes, it was cooled to room temperature. The crystals precipitated was separated by filtration and dried under vacuo to afford 3.72 g of the title compound having mp. 189.5°-193° C.

후처리

  1. customwere removed through a Dean-Stark's water
  2. temperatureWhile heating, to the mixture
  3. temperatureafter the resulted mixture was refluxed for forty minutes
  4. customThe crystals precipitated
  5. customwas separated by filtration
  6. customdried under vacuo

출처 및 근거

ORD 기록
ord-d9b0f5ada74b43739e4425787d83cdc9
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04943314

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