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

HRID 1602456노트

반응식

HRID 1602456 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, 5 Apr 89) (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-7b8bf217a0c344778d0df40b5fe640df
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05981571

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