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Ethanolamine → 7-beta-D-galactopyranosyloxycoumarin-4-acetic acid-(2-hydroxyethyl)amide

HRID 610661
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HRID 610661 반응식
C([O:4][C@@H:5]1[C@@H:10]([O:11]C(=O)C)[C@@H:9]([O:15]C(=O)C)[C@@H:8]([CH2:19][O:20]C(=O)C)[O:7][C@H:6]1[O:24][C:25]1[CH:34]=[C:33]2[C:28]([C:29]([CH2:36][C:37]([O-])=[O:38])=[CH:30][C:31](=[O:35])[O:32]2)=[CH:27][CH:26]=1)(=O)C.[CH2:40]([CH2:42][NH2:43])[OH:41]>C(Cl)Cl.CO.CCOCC>[OH:41][CH2:40][CH2:42][NH:43][C:37](=[O:38])[CH2:36][C:29]1[C:28]2[C:33](=[CH:34][C:25]([O:24][C@@H:6]3[O:7][C@H:8]([CH2:19][OH:20])[C@H:9]([OH:15])[C@H:10]([OH:11])[C@H:5]3[OH:4])=[CH:26][CH:27]=2)[O:32][C:31](=[O:35])[CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 700EthanolamineHCID 867549227-(2,3,4,6-tetra-O-acetyl-beta-D-galactopyranosyloxy)coumarin-4-acetate2회

생성물 1

HCID 99541407-beta-D-galactopyranosyloxycoumarin-4-acetic acid-(2-hydroxyethyl)amide수율 37.1%

시약·촉매·용매 3

HCID 887Methanol용매HCID 3283Diethyl Ether용매
HCID 6344
Dichloromethane
용매

실험 절차

43 g (0.076 moles) of 7-(2,3,4,6-tetra-O-acetyl-β-D-galactopyranosyloxy)coumarin-4-acetate (i.e. compound 1 prepared as described in Scheme 1) was dissolved in 430 ml of methylene chloride in a 1 liter RB flask. 43 ml (0.712 moles) of ethanolamine was dissolved in 43 ml of methanol and added to the above solution. The solution was stirred at room temperature for 60 hrs and the resulting solid residue was filtered and washed with 50 ml of methylene chloride. The solid was suspended in 250 ml of methanol and stored in the freezer for 12 hrs. The solid was filtered again and suspended in 700 ml of methanol and refluxed for 30 min. The cloudy suspension was cooled to room temperature, then further cooled in an ice bath and filtered. The wet solid thus obtained was suspended in 200 ml of ether and stirred for 30 min., then filtered and vacuum dried at room temperature to give 12 g of an off-white solid. The yield was 37%. The structure was confirmed by 1H NMR and MS (as in Example 1).

후처리

  1. additionadded to the above solution
  2. filtrationthe resulting solid residue was filtered
  3. washwashed with 50 ml of methylene chloride
  4. waitstored in the freezer for 12 hrs
  5. filtrationThe solid was filtered again
  6. temperaturerefluxed for 30 min
  7. temperatureThe cloudy suspension was cooled to room temperature
  8. temperaturefurther cooled in an ice bath
  9. filtrationfiltered
  10. customThe wet solid thus obtained
  11. stirringstirred for 30 min.
  12. filtrationfiltered
  13. customvacuum dried at room temperature

출처 및 근거

ORD 기록
ord-81773609d59c4a23bdcf5304d2876e25
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998593

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