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N-bromobutanimide → HCID 86701093, 화합물

HRID 1396232
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HRID 1396232 반응식
[CH3:1][O:2][C:3]1[CH:34]=[CH:33][C:6]([CH2:7][O:8][C@@H:9]2[C@@H:17]([CH2:18][OH:19])[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:20]([CH3:22])[CH3:21])[S:14]3)[C@H:10]2[O:23][CH2:24][C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:5][CH:4]=1.C1C(=O)N(Br)C(=O)C1>CCCC[N+](CCCC)(CCCC)CCCC.[Br-].ClCCl.O.CC1(C)N([O])C(C)(C)CCC1>[CH3:22][N:20]([CH3:21])[C:13]1[S:14][C@H:15]2[O:16][C@H:17]([CH:18]=[O:19])[C@@H:9]([O:8][CH2:7][C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:34][CH:33]=3)[C@H:10]([O:23][CH2:24][C:25]3[CH:26]=[CH:27][C:28]([O:31][CH3:32])=[CH:29][CH:30]=3)[C@H:11]2[N:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 67184N-bromobutanimideHCID 69083734HCID 69083734, 화합물

생성물 1

HCID 86701093HCID 86701093, 화합물수율 75%

시약·촉매·용매 4

HCID 74236Tetrabutylammonium Bromide촉매HCID 2724126Tempo촉매HCID 962Water
용매
HCID 6344Dichloromethane용매

실험 절차

To a mixture of ((3aR,5R,6S,7R,7aR)-6,7-bis(4-methoxybenzyloxy)-2-(dimethylamino)-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]thiazol-5-yl)methanol (500 mg, 1.0 mmol), TBAB (16.5 mg, 0.05 mmol), KHCO3 (461 mg, 4.6 mmol) and TEMPO (8 mg, 0.05 mmol) in dichloromethane (25 mL) and H2O (5 mL) was added NBS (201 mg, 1.13 mmol) at 15° C. After stirred for 30 min, the reaction mixture was quenched by saturated Na2SO3 (5 mL). The organic layer was dried over anhydrous magnesium sulfate and condensed to provide a residue, which was purified by silica gel column, eluted with 20-30% ethyl acetate in dichloromethane to give compound 11 as a yellow syrup (320 mg, 75% pure). (ES, m/z): [M+H]+ 487.0. 1H NMR (300 MHz, CDCl3) δ 9.61 (s, 1H), 7.22-7.34 (m, 4H), 6.83-6.92 (m, 4H), 6.11-6.13 (d, J=6.0 Hz, 1H), 4.17-4.67 (m, 8H), 3.83 (s, 6H), 3.00-3.04 (s, 6H).

후처리

  1. customthe reaction mixture was quenched by saturated Na2SO3 (5 mL)
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate and condensed
  3. customto provide a residue, which
  4. customwas purified by silica gel column
  5. washeluted with 20-30% ethyl acetate in dichloromethane

출처 및 근거

ORD 기록
ord-1a329fb0e9b64d12885c4343129cd2c5
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901087B2

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