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Sodium hydride → HCID 14819342, 화합물

HRID 330273
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HRID 330273 반응식
[H-].[Na+].[C:3]([CH2:5]P(=O)(OCC)OCC)#[N:4].[Cl:14][C:15]1[C:23]2[O:22][CH2:21][C:20](=O)[C:19]=2[CH:18]=[CH:17][CH:16]=1>C1COCC1>[Cl:14][C:15]1[C:23]2[O:22][CH:21]=[C:20]([CH2:5][C:3]#[N:4])[C:19]=2[CH:18]=[CH:17][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 75676Diethyl (cyanomethyl)phosphonateHCID 148193417-Chloro-3(2H)-benzofuranone

생성물 1

HCID 14819342HCID 14819342, 화합물수율 97.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
0 °C

실험 절차

To a stirred suspension of NaH 50% dispersion in mineral oil, washed with hexane; 1.82 g, 0.0378 mol) in THF (70 mL) was added a solution of diethyl cyanomethylphosphonate (6.7 g, 0.0378 mol) in THF (30 mL) dropwise over 20 minutes. After 20 minutes, the mixture was cooled to 0° C. and a solution of 7-chlorobenzofuran-3-one (5.8 g, 0.0344 mol) in THF (80 mL) was added dropwise over 30 minutes. The cooling bath was removed and stirring was continued at room temperature overnight. H2O (400 mL) and ether were added. The organic phase was washed with saturated aqueous NaCl, dried (MgSO4), and concentrated to give a red solid (6.4 g, 97%).

후처리

  1. washwashed with hexane
  2. customThe cooling bath was removed
  3. waitwas continued at room temperature overnight
  4. additionH2O (400 mL) and ether were added
  5. washThe organic phase was washed with saturated aqueous NaCl
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-73e85f9b94f14ff48c00cb054b74ab0b
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04895860

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