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Formamide → HCID 15005406, 화합물

HRID 892774
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HRID 892774 반응식
[CH:1]([NH2:3])=[O:2].Br[CH:5]([C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1)[C:6](=O)[CH3:7].C(=O)(O)[O-].[Na+]>ClCCl>[C:13]([C:12]1[CH:15]=[CH:16][C:9]([C:5]2[O:2][CH:1]=[N:3][C:6]=2[CH3:7])=[CH:10][CH:11]=1)#[N:14]
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참가 물질

5

반응물 3

HCID 713FormamideHCID 516892Sodium BicarbonateHCID 15005405HCID 15005405, 화합물

생성물 1

HCID 15005406HCID 15005406, 화합물수율 63.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred, two-phase mixture of formamide (0.6 ml, 15 mmol) and 4-(1-bromo-2-oxopropyl)benzonitrile (0.8 g, 3.4 mmol) was heated to 120° for 2 hours. After cooling, dichloromethane (15 ml) and saturated aqueous sodium bicarbonate (10 ml) were added, the organic phase was separated, dried (magnesium sulphate) and the solvent removed under reduced pressure to yield 0.4 g of an amorphous yellow solid. The product was purified by silica gel chromatography, eluting with dichloromethane to yield the title compound (0.29 g, 47%) as a pale yellow solid, m.p. 120°-121° C.

후처리

  1. temperaturewas heated to 120° for 2 hours
  2. temperatureAfter cooling
  3. customthe organic phase was separated
  4. dry with materialdried (magnesium sulphate)
  5. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-432de15b6c1e4ef09eeec18ab8da8498
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05120747

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