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Sulfuric Acid → HCID 59730230, 화합물

HRID 925224
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HRID 925224 반응식
N[C:2]1[CH:18]=[CH:17][C:5]2[CH2:6][CH2:7][N:8]([C:11](=[O:16])[C:12]([F:15])([F:14])[F:13])[CH2:9][CH2:10][C:4]=2[CH:3]=1.[OH:19]S(O)(=O)=O.N([O-])=O.[Na+]>O>[F:13][C:12]([F:15])([F:14])[C:11]([N:8]1[CH2:9][CH2:10][C:4]2[CH:3]=[C:2]([OH:19])[CH:18]=[CH:17][C:5]=2[CH2:6][CH2:7]1)=[O:16]
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참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 18943538HCID 18943538, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 59730230HCID 59730230, 화합물

시약·촉매·용매 1

HCID 962Water용매3회

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온도
70 °C

실험 절차

Into a 250 ml flask, the product of step (c) (2 g, 7.75 mmol) dissolved in water (8.5 ml) and concentrated H2SO4 (1.5 ml) was added. The stirred mixture was heated to 70° C., followed by the addition of a solution NaNO2 (615 mg, 8.91 mmol) in water (20 ml). The reaction mixture was stirred at 70° C. for 1 hour. The mixture was then allowed to cool to room temperature and diluted with water (50 ml). The aqueous mixture was extracted with EtOAc (3×). The combined EtOAc extracts were washed with brine, dried over Na2SO4, and solvent evaporated in vacuo to give the sub-title compound as a brown solid (1.8 g) that was used without further purification. MS: ESI (positive): 260 (M+H).

후처리

  1. temperatureto cool to room temperature
  2. extractionThe aqueous mixture was extracted with EtOAc (3×)
  3. washThe combined EtOAc extracts were washed with brine
  4. dry with materialdried over Na2SO4, and solvent
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-9efc7799939a4bf59895cb943dcdfbbf
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284277B2

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