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Hydrogen Peroxide → HCID 178513609, 화합물

HRID 1524864
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HRID 1524864 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[C:11]([CH:14]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:15]([O:17]C)=[O:16])[NH:12][CH:13]=2)=[CH:5][CH:4]=1)#[N:2].C(=O)([O-])[O-:27].[K+].[K+].OO.[O-2].[Mg+2]>CS(C)=O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:10]=[C:11]([CH:14]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:15]([OH:17])=[O:16])[NH:12][CH:13]=2)=[CH:7][CH:8]=1)(=[O:27])[NH2:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 6850729Magnesium monoxideHCID 178499804HCID 178499804, 화합물

생성물 1

HCID 178513609HCID 178513609, 화합물수율 67%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
2.5 °C

실험 절차

The product from Example 56 Part A (0.99 g, 3.0 mmol) was dissolved in 10 mL of DMSO. Potassium carbonate (1.24 g, 9.0 mmol) was added. The mixture was cooled to 0-5° C. and 30% H2O2 (3.18 mL of 30% aqueous solution) was added, followed by magnesium oxide (0.24 g, 15 mmol). The cooling bath was removed and the mixture was stirred at RT under N2 for 4 h. The mixture was filtered to remove inorganic material. Water (30 mL) was added to the filtrate and the resulting mixture was stirred at rt for 40 min. The mixture was acidified with 1N HCl to pH 5. The precipitate formed was filtered and dried to afford 0.67 g of the acid (67%). MS 336.30 (M+H)+.

후처리

  1. customThe cooling bath was removed
  2. filtrationThe mixture was filtered
  3. customto remove inorganic material
  4. additionWater (30 mL) was added to the filtrate
  5. stirringthe resulting mixture was stirred at rt for 40 min
  6. customThe precipitate formed
  7. filtrationwas filtered
  8. customdried

출처 및 근거

ORD 기록
ord-e8046466f7c9498b85c243d04e4247e2
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079860B2

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