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Formamide → HCID 15005406, 화합물

HRID 1460314
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HRID 1460314 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]
참가 물질실험 절차후처리출처 및 근거반응 노트

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.

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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-b3fb7e4c094a4ddb91ecb6f8f9c030b0
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05070205

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