Acetone → 7-Hydroxymethylcoumarin

HRID 1090760노트

반응식

HRID 1090760 반응식
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

참가 물질

5

반응물 3

HCID 180AcetoneHCID 2641197-(Bromomethyl)-2h-chromen-2-oneHCID 516892Sodium Bicarbonate

생성물 1

HCID 150282577-Hydroxymethylcoumarin

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10bd2cab9400439a9ff0ac45b562a8d9
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05082934

반응 노트

불러오는 중…