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Sodium Bicarbonate → HCID 11716529, 화합물

HRID 563050
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HRID 563050 반응식
FC(F)(F)C(O)=O.[NH2:8][C@@H:9]([CH2:13][O:14][C:15]([O:17][C:18]1[C:23]([CH:24]([CH3:26])[CH3:25])=[CH:22][CH:21]=[CH:20][C:19]=1[CH:27]([CH3:29])[CH3:28])=[O:16])[C:10]([OH:12])=[O:11].C(=O)(O)[O-].[Na+]>O.CC#N>[NH2:8][C@@H:9]([CH2:13][O:14][C:15]([O:17][C:18]1[C:23]([CH:24]([CH3:25])[CH3:26])=[CH:22][CH:21]=[CH:20][C:19]=1[CH:27]([CH3:29])[CH3:28])=[O:16])[C:10]([OH:12])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 67005495HCID 67005495, 화합물

생성물 1

HCID 11716529HCID 11716529, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

To a stirred solution of compound (8) in H2O and MeCN (20/1 v/v) was added a saturated aqueous sodium bicarbonate solution dropwise. The pH of this reaction mixture was monitored closely and the desired product precipitated as a white solid after the pH was adjusted to 7. The mixture was filtered and the title compound (3) was collected and dried in vacuo. 1H-NMR (400 MHz, CDCl3): δ 7.15-7.22 (m, 3H), 4.64-4.68 (dd, J=11.6, 3.2 Hz, 1H), 4.55-4.60 (dd, J=11.6, 6.8 Hz, 1H), 3.28-3.30 (dd, J=6.8, 3.2 Hz, 1H), 2.99-3.04 (m, 2H), 1.18-1.19 (d, J=6.4 Hz, 12H). MS (ESI) m/z 310.3 (M+H)+.

후처리

  1. customthe desired product precipitated as a white solid after the pH
  2. filtrationThe mixture was filtered
  3. customthe title compound (3) was collected
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-baa0a71e6c3a4a8da93e74d38bac0319
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08067455B2

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