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Formic Acid → HCID 14685751, 화합물

HRID 1088804
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인쇄 미리보기

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HRID 1088804 반응식
[O:1]=[C:2]1[O:7][CH2:6][C:5]2[CH:8]=[CH:9][CH:10]=[C:11]3[CH:12]([NH:15][CH2:16][CH:17]=[CH2:18])[CH2:13][CH2:14][N:3]1[C:4]=23.[CH:19](O)=O>C=O>[O:1]=[C:2]1[O:7][CH2:6][C:5]2[CH:8]=[CH:9][CH:10]=[C:11]3[CH:12]([N:15]([CH3:19])[CH2:16][CH:17]=[CH2:18])[CH2:13][CH2:14][N:3]1[C:4]=23
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 14685750HCID 14685750, 화합물

생성물 1

HCID 14685751HCID 14685751, 화합물

시약·촉매·용매 1

HCID 712Formaldehyde용매

반응 조건

온도
90 °C

실험 절차

6,7-Dihydro-3-oxo-7-allylamino-1H,3H,5H-pyrido[3,2,1-ij][3,1]benzoxazine (5.86 g) was dissolved in a solution of formic acid (7 ml) and 35% formalin (7 ml), and the solution was stirred for 2 hours at 90° C. Formic acid and formalin were distilled off under reduced pressure, and to this mixture were added ice water and dichloromethane, and the mixture was adjusted to alkalinic with sodium carbonate. The mixture was extracted with dichloromethane, dried over anhydrous magnesium sulfate, and distilled off to give 6,7-dihydro-3-oxo-7-(N-methyl-N-allylamino)- 1H,3H,5H-pyrido[3,2,1-ij][3,1]benzoxazine (5.90 g).

후처리

  1. distillationFormic acid and formalin were distilled off under reduced pressure
  2. additionto this mixture were added ice water and dichloromethane
  3. extractionThe mixture was extracted with dichloromethane
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationdistilled off

출처 및 근거

ORD 기록
ord-7e7b224a2ee84c50853155c269fa3520
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04963566

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