Chloride → 1,2-Benzenediol, 4-(3-hydroxypropyl)-

HRID 909698

反応式

HRID 909698 の反応式
O[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([OH:12])[C:8](=[CH:10][CH:11]=1)[OH:9])=O.[Na].[Cl-].[H][H].[CH3:17][OH:18]>[Pd].O>[CH:11]1[C:5]([CH2:3][CH2:2][CH2:17][OH:18])=[CH:6][C:7]([OH:12])=[C:8]([OH:9])[CH:10]=1

参加物

8

反応物 5

HCID 312ChlorideHCID 887MethanolHCID 5360545SodiumHCID 221344442-Hydroxy-3′,4′-dihydroxyacetophenone2 回HCID 178418361HCID 178418361、化合物

生成物 1

HCID 112174641,2-Benzenediol, 4-(3-hydroxypropyl)-

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒2 回

実験手順

In a reactor as described in Example 5 well dried samples of 1.5 g of 4-hydroxyacetyl-catechol with very low sodium and chloride content (<0.15%) were hydrogenated in the presence or absence of added water. All reactions were run with 0.15 g Pd/C (10%) in 30 ml of solvent at 5 bar and 40° C. at least to the end of hydrogen uptake. The catalyst was filtered off and washed with ethyl acetate. The solutions were concentrated and the residues analyzed quantitatively. The results are summarized in Table 3 snowing the influence of the added water. The starting material was totally consumed in every experiment at the end. The data shows that the result is clearly improved at a relation of 1 mol water added per 3 moles of 4-hydroxyacetyl-catechol and is even better at a relation of 1/1 mole. The lower suitability of methanol as solvent is also demonstrated.

後処理

  1. filtrationThe catalyst was filtered off
  2. washwashed with ethyl acetate
  3. concentrationThe solutions were concentrated
  4. customThe starting material was totally consumed in every experiment at the end

出典と根拠

ORDレコード
ord-bce44eb78c57497384c287ead8007012
出典データセット
uspto-grants-2011_09
特許番号
US08017815B2

関連ノート

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