Acetic Acid → HCID 14279665, 화합물

HRID 2291772노트

반응식

HRID 2291772 반응식
[NH2:1][C:2]1[C:3]([F:16])=[CH:4][C:5]2[O:10][CH2:9][C:8](=[O:11])[N:7]([CH2:12][C:13]#[N:14])[C:6]=2[CH:15]=1.[C:17]1(=O)[O:22][C:20](=[O:21])[CH:19]2[CH2:23][CH2:24][CH:25]=[CH:26][CH:18]12.C(O)(=O)C>O>[C:13]([CH2:12][N:7]1[C:6]2[CH:15]=[C:2]([N:1]3[C:20](=[O:21])[C:19]4[CH2:23][CH2:24][CH2:25][CH2:26][C:18]=4[C:17]3=[O:22])[C:3]([F:16])=[CH:4][C:5]=2[O:10][CH2:9][C:8]1=[O:11])#[N:14]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 127266013a,4,5,7a-Tetrahydro-2-benzofuran-1,3-dioneHCID 14347817HCID 14347817, 화합물

생성물 1

HCID 14279665HCID 14279665, 화합물수율 73.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

6-amino-4-cyanomethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-one (0.5 g), tetrahydrophthalic anhydride (0.38 g) and acetic acid (10 ml) were mixed with each other, then the mixture was refluxed under heating for 3 hours. After the liquor was allowed to cool, it was added to water (40 ml), and separating crystals were collected by filtration, and then the crystals were dissolved in dichloromethane (30 ml). The dichloromethane solution was washed with a saturated solution of sodium bicarbonate, and water, in that order, and then dehydrated with anhydrous sodium sulfate, and subsequently concentrated. Separated crystals were washed with a small amount of ether to give the desired 2-[4-cyanomethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-on 6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (0.59 g). mp. 227°-229° C.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating for 3 hours
  3. temperatureto cool
  4. customseparating crystals
  5. filtrationwere collected by filtration
  6. dissolutionthe crystals were dissolved in dichloromethane (30 ml)
  7. washThe dichloromethane solution was washed with a saturated solution of sodium bicarbonate, and water, in that order
  8. concentrationsubsequently concentrated
  9. customSeparated crystals
  10. washwere washed with a small amount of ether

출처 및 근거

ORD 기록
ord-9fa03911a1d5483792a705c41cbef472
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04798620

반응 노트

불러오는 중…