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Sodium hydride → HCID 11629847, 화합물

HRID 2067090
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HRID 2067090 반응식
[H-].[Na+].[F:3][C:4]1[C:12]2[O:11][C:10](=[O:13])[NH:9][C:8]=2[CH:7]=[CH:6][CH:5]=1.Br[CH2:15][C:16]([NH2:18])=[O:17]>CN(C=O)C>[F:3][C:4]1[C:12]2[O:11][C:10](=[O:13])[N:9]([CH2:15][C:16]([NH2:18])=[O:17])[C:8]=2[CH:7]=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 696322-BromoacetamideHCID 21989976HCID 21989976, 화합물

생성물 1

HCID 11629847HCID 11629847, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a three neck flask, fitted with a magnetic stirrer, under inert atmosphere, NaH (in oil, 60 w/w, 1.8 g, 45.15 mmol) is carefully added by portion into a solution of 7-fluoro-1,3-benzoxazol-2(3H)-one 2 (5.76 g, 37.62 mmol) in dried DMF (80 ml) at 0° C. After 0.25 h, 2-bromo-acetamide (6.22 g, 45.15 mmol) is added. The reaction mixture is stirred for 1 h at room temperature, quenched with water, concentrated in vacuo and the residue is recrystallized in EtOH/H2O (80/20 (v/v)) to afford 2-(7-fluoro-2-oxo-1,3-benzoxazol-3(2H)-yl)acetamide.

후처리

  1. customquenched with water
  2. concentrationconcentrated in vacuo
  3. customthe residue is recrystallized in EtOH/H2O (80/20 (v/v))

출처 및 근거

ORD 기록
ord-f62a90a0c3424176b0b988b78348dbd4
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08293775B2

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