Ethyl Acetate → HCID 14014835, 화합물

HRID 727941

반응식

HRID 727941 반응식
O.[CH:2]12[CH2:8][CH:5]([NH:6][CH2:7]1)[CH2:4][N:3]2[C:9]1[CH:18]=[C:17]2[C:12]([C:13](=[O:30])[C:14]([C:27]([OH:29])=[O:28])=[CH:15][N:16]2[C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=2[F:26])=[CH:11][C:10]=1[F:31].C(=O)(O)[O-].[Ca+2].C(=O)(O)[O-].Br[CH2:42][C:43]1[O:44][C:45](=[O:49])[O:46][C:47]=1[CH3:48].C(OCC)(=O)C>CN(C=O)C.O>[F:26][C:20]1[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:19]=1[N:16]1[C:17]2[C:12](=[CH:11][C:10]([F:31])=[C:9]([N:3]3[CH2:4][CH:5]4[CH2:8][CH:2]3[CH2:7][N:6]4[CH2:42][C:43]3[O:44][C:45](=[O:49])[O:46][C:47]=3[CH3:48])[CH:18]=2)[C:13](=[O:30])[C:14]([C:27]([OH:29])=[O:28])=[CH:15]1

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 10176262Calcium bicarbonateHCID 107741414-(Bromomethyl)-5-methyl-1,3-dioxol-2-oneHCID 67927890HCID 67927890, 화합물

생성물 1

HCID 14014835HCID 14014835, 화합물수율 27.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To 188 mg (0.434 m Mol) of 7-(2,5-diazabicyclo(2.2.1)hept-2-yl)-6-fluoro-1-(2,4-difluorophenyl)-1,4-di-hydro-4-oxoquinoline-3-carboxylic acid monohydrate (Example 11) was suspended in 20 ml dry DMF was added 96 mg (0.95 m Mol) anhydrous calcium bicarbonate and 92 mg (0.48 m Mol) 4-bromomethyl-5-methyl-1,3-dioxolen-2-one. The resultant suspension was stirred at room temperature for 10 hrs. Then the suspension was treated with 150 ml of ethyl acetate and 50 ml of water. The organic phase was separated and washed with 5×30 ml water, dried over sodium sulfate, filtered the volatiles were removed at room temperature under reduced pressure. Recrystallization from ethyl acetate gave 63 mg (27.5%) of the desired material.

후처리

  1. customThe organic phase was separated
  2. washwashed with 5×30 ml water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered the volatiles
  5. customwere removed at room temperature under reduced pressure
  6. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-91c076c09db74192bcdea3de1c3ea8e2
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045549

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