Acetone → 7-Hydroxymethylcoumarin

HRID 1090760ノート

反応式

HRID 1090760 の反応式
CC(C)=[O:3].Br[CH2:6][C:7]1[CH:16]=[C:15]2[C:10]([CH:11]=[CH:12][C:13](=[O:17])[O:14]2)=[CH:9][CH:8]=1.C(=O)(O)[O-].[Na+]>O>[OH:3][CH2:6][C:7]1[CH:16]=[C:15]2[C:10]([CH:11]=[CH:12][C:13](=[O:17])[O:14]2)=[CH:9][CH:8]=1

参加物

5

実験手順

To a 1:1 mixture of acetone and water (560 ml) was added 7-bromomethy1coumarin (7.0 g, 29.3 mmol). The resulting suspension was refluxed for 48 hrs at which time the reaction mixture became a clear solution. The solution was then cooled and neutralized with sodium bicarbonate (2.4 g, 29.3 mmol) and concentrated in vacuo to about 65 ml. A thick mass of crystals resulted. The crystals were collected by filtration to yield 5.27 g of product after drying in vacuo (100% of theory). The melting point was 116°-117° C.

後処理

  1. temperatureThe resulting suspension was refluxed for 48 hrs at which time the reaction mixture
  2. temperatureThe solution was then cooled
  3. concentrationconcentrated in vacuo to about 65 ml
  4. customA thick mass of crystals resulted
  5. filtrationThe crystals were collected by filtration

出典と根拠

ORDレコード
ord-10bd2cab9400439a9ff0ac45b562a8d9
出典データセット
uspto-grants-1992_01
特許番号
US05082934

反応ノート

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