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Hydrogen Peroxide → HCID 178513609、化合物

HRID 1524864
ノート
印刷プレビュー

反応式

HRID 1524864 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 6850729Magnesium monoxideHCID 178499804HCID 178499804、化合物

生成物 1

HCID 178513609HCID 178513609、化合物収率 67%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
2.5 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-e8046466f7c9498b85c243d04e4247e2
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09079860B2

反応ノート

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