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Diethyl (cyanomethyl)phosphonate → HCID 66824449, 화합물

HRID 1692926
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HRID 1692926 반응식
CC(C)([O-])C.[K+].[C:7]([CH2:9]P(=O)(OCC)OCC)#[N:8].[F:18][CH2:19][C:20]1([C:25]#[N:26])[CH2:23][C:22](=O)[CH2:21]1>O1CCCC1>[C:7]([CH:9]=[C:22]1[CH2:23][C:20]([CH2:19][F:18])([C:25]#[N:26])[CH2:21]1)#[N:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 75676Diethyl (cyanomethyl)phosphonateHCID 23665647Potassium tert-butoxideHCID 66824419HCID 66824419, 화합물

생성물 1

HCID 66824449HCID 66824449, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a solution of 1.0 M of potassium tert-butoxide in tetrahydrofuran (2.15 mL) at 0° C. was added dropwise a solution of diethyl cyanomethylphosphonate (0.364 mL, 0.00225 mol) in tetrahydrofuran (4 mL, 0.04 mol). The reaction was warmed to rt and then cooled to 0° C. again. To the reaction mixture was added a solution of 1-(fluoromethyl)-3-oxocyclobutanecarbonitrile (0.260 g, 0.00204 mol) in tetrahydrofuran (2 mL, 0.02 mol). The reaction was allowed to warm up to rt and stirred at rt overnight. After quenching with water, the mixture was extracted with ether. The combined organic layers were washed with water then brine, dried, and evaporated to dryness. The crude mixture was used directly in next step.

후처리

  1. temperaturecooled to 0° C. again
  2. temperatureto warm up to rt
  3. customAfter quenching with water
  4. extractionthe mixture was extracted with ether
  5. washThe combined organic layers were washed with water
  6. dry with materialbrine, dried
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-94353a1e595445cc99ad29277304e379
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158616B2

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