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Hydrochloric Acid → HCID 17816448、化合物

HRID 2249688
ノート
印刷プレビュー

反応式

HRID 2249688 の反応式
[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[O:15][CH2:16][CH2:17][CH:18]([CH3:20])[CH3:19])[CH:10]=[O:11])[CH2:2][CH:3]([CH3:5])[CH3:4].P([O-])(O)(O)=[O:22].[Na+].Cl([O-])=O.[Na+].Cl>C(#N)C.O.OO.C(Cl)(Cl)Cl>[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[O:15][CH2:16][CH2:17][CH:18]([CH3:20])[CH3:19])[C:10]([OH:22])=[O:11])[CH2:2][CH:3]([CH3:5])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 17816516HCID 17816516、化合物HCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

生成物 1

HCID 17816448HCID 17816448、化合物収率 94.6%

試薬・触媒・溶媒 4

HCID 784Hydrogen Peroxide溶媒
HCID 962
Water
溶媒
3 回
HCID 6212Chloroform溶媒
HCID 6342Acetonitrile溶媒

実験手順

In 30 ml of acetonitrile is dissolved 3.0 g of 3,4-diisopentyloxybenzaldehyde, to which are successively added at ambient temperature a solution of 4.5 g of sodium dihydrogenphosphate in 15 ml of water and 1.8 ml of 30% aqueous hydrogen peroxide. Then, a solution of 2.0 g of sodium chlorite in 30 ml of water is dropwise added thereto at 5-10° C., and the mixture thus obtained is stirred at ambient temperature for 3.5 hours. Chloroform and water are added to the reaction mixture, pH is adjusted to 2 with 6 mol/L hydrochloric acid, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. Thus, 3.0 g of 3,4-diisopentyloxybenzoic acid is obtained as a white solid product.

後処理

  1. customat 5-10° C., and the mixture thus obtained
  2. customthe organic layer is separated
  3. customThe organic layer thus obtained
  4. washis washed with water and saturated aqueous solution of sodium chloride successively
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-114473b6126648bd8b7830208eda3f1e
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

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