Levulinic Acid → HCID 86734554, 화합물

HRID 597050

반응식

HRID 597050 반응식
[CH3:1][C:2]([CH2:4][CH2:5][C:6]([OH:8])=[O:7])=[O:3].Cl.[Cl:10][C:11]1[CH:20]=[C:19]2[C:14]([C:15]([N:21]([C:25]3[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=3)N=CC)=[N:16][CH:17]=[N:18]2)=[CH:13][CH:12]=1>O>[OH2:3].[CH3:1][C:2]1[N:21]([C:15]2[C:14]3[C:19](=[CH:20][C:11]([Cl:10])=[CH:12][CH:13]=3)[N:18]=[CH:17][N:16]=2)[C:25]2[C:26]([C:4]=1[CH2:5][C:6]([OH:8])=[O:7])=[CH:27][C:28]([O:31][CH3:32])=[CH:29][CH:30]=2

참가 물질

4

반응물 2

HCID 11579Levulinic AcidHCID 86734555acetaldehyde N1-(7-chloroquinazolin-4-yl)p-methoxyphenylhydrazone hydrochloride

생성물 1

HCID 86734554HCID 86734554, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of laevulinic acid (15g.) and acetaldehyde N1 -(7-chloroquinazolin-4-yl)-p-methoxyphenylhydrazone hydrochloride (3.3g.) was heated at 95°-100° C. for 18 hours. The mixture was poured into water (ca 300ml.), and the precipitated pale yellow solid was collected by filtration and dissolved in a mixture of water (80ml.) and ammonia solution (specific gravity 0.88, ca 5ml.). The solution was washed with ethyl acetate (2 × 25ml.). Addition of sodium chloride (ca 10g.) to the aqueous phase caused a yellow solid to precipitate. This was collected by filtration, and then dissolved in water. The solution was acidified with glacial acetic acid until precipitation was complete. The mixture was filtered to give, as solid residue, 2-methyl-5-methoxy-1-(7-chloroquinazolin-4-yl)indol-3-ylacetic acid monohydrate, m.p. 98°-100° C.

후처리

  1. temperaturewas heated at 95°-100° C. for 18 hours
  2. filtrationthe precipitated pale yellow solid was collected by filtration
  3. dissolutiondissolved in a mixture of water (80ml.) and ammonia solution (specific gravity 0.88, ca 5ml.)
  4. washThe solution was washed with ethyl acetate (2 × 25ml.)
  5. additionAddition of sodium chloride (ca 10g.) to the aqueous phase
  6. customto precipitate
  7. filtrationThis was collected by filtration
  8. dissolutiondissolved in water
  9. customThe solution was acidified with glacial acetic acid until precipitation
  10. filtrationThe mixture was filtered

출처 및 근거

ORD 기록
ord-157e2c242f784cbaac7562b73481385d
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012513

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