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1,3-Dioxolane, 4-[(2,4-dinitrophenoxy)methyl]-2,2-dimethyl- → HCID 11128347, 화합물

HRID 1737126
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HRID 1737126 반응식
[N+:1]([C:4]1[CH:18]=[C:17]([N+:19]([O-])=O)[CH:16]=[CH:15][C:5]=1[O:6][CH2:7][CH:8]1[CH2:12][O:11][C:10]([CH3:14])([CH3:13])[O:9]1)([O-])=O.[H][H]>[Pd].CO>[NH2:1][C:4]1[CH:18]=[C:17]([NH2:19])[CH:16]=[CH:15][C:5]=1[O:6][CH2:7][CH:8]1[CH2:12][O:11][C:10]([CH3:13])([CH3:14])[O:9]1
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참가 물질

5

반응물 2

HCID 111092861,3-Dioxolane, 4-[(2,4-dinitrophenoxy)methyl]-2,2-dimethyl-HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 11128347HCID 11128347, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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온도
5 °C

실험 절차

215 ml of methanol are introduced into a 0.7 l autoclave, 85.3 g (0.3 mole) of 4-(2,4-dinitrophenoxymethyl)-2,2-dimethyl-1,3-dioxolane (step a) are dissolved therein and 0.6 g of palladium on active carbon 10% (Degussa) is added. After the autoclave has been closed and blanketed with nitrogen, hydrogenation is carried out under a pressure of 4 bar and at a temperature of 35 to 40° C. until no more hydrogen is taken up. 1.3 g of active carbon is added under nitrogen to the warm solution and the catalyst is filtered off. 42 g of 70% sulfuric acid are added dropwise to the solution while cooling with ice at 5° C. The product precipitated is filtered off under suction, washed with methanol and dried.

후처리

  1. dissolutionare dissolved
  2. customAfter the autoclave has been closed
  3. addition1.3 g of active carbon is added under nitrogen to the warm solution
  4. filtrationthe catalyst is filtered off
  5. addition42 g of 70% sulfuric acid are added dropwise to the solution
  6. customThe product precipitated
  7. filtrationis filtered off under suction
  8. washwashed with methanol
  9. customdried

출처 및 근거

ORD 기록
ord-8f0973d921b74fde98f804f1e8baf2ee
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05961668

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