Malonic Acid → (E)-3-(2,3-dihydrobenzo[b][1,4]dioxin-5-yl)acrylic acid

HRID 1107554노트

반응식

HRID 1107554 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]=O)[C:5]=2[O:4][CH2:3][CH2:2]1.C(O)(=O)[CH2:14][C:15]([OH:17])=[O:16].N1CCCC1>N1C=CC=CC=1>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10](/[CH:11]=[CH:14]/[C:15]([OH:17])=[O:16])[C:5]=2[O:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 867Malonic AcidHCID 31268PyrrolidineHCID 27950332,3-Dihydro-1,4-benzodioxine-5-carbaldehyde

생성물 1

HCID 5343159(E)-3-(2,3-dihydrobenzo[b][1,4]dioxin-5-yl)acrylic acid

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2,3-dihydrobenzodioxin-5-carboxaldehyde (Morishima, et al., Eur. Pat. Appl. 309,766, Apr. 5, 1989) (9.25 g, 56.4 mmol), malonic acid (11.73 g, 112.8 mmol), pyrrolidine (1 mL), and pyridine (25 mL) was heated to reflux for 2 hr, cooled, and then poured into ice water (300 mL). The white precipitate was filtered, washed with 1N HCl, and air dried (9.83 g, 84.6%).

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hr
  3. temperaturecooled
  4. filtrationThe white precipitate was filtered
  5. washwashed with 1N HCl, and air
  6. customdried (9.83 g, 84.6%)

출처 및 근거

ORD 기록
ord-04cf1a436de6409ca69f7fb1cfa8a35d
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06060506

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