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Ethanol → HCID 178476779, 화합물

HRID 482639
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HRID 482639 반응식
[C:1]1([P:7](Cl)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:10]([OH:12])[CH3:11].N1C=CC=CC=1.[OH2:19]>CCOCC>[C:1]1([PH:7](=[O:19])[O:12][CH2:10][CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 962WaterHCID 1049Pyridine2회HCID 12573Phenyl phosphorus dichloride

생성물 1

HCID 178476779HCID 178476779, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of phenylphosphonous dichloride (66 g, 0.37 mol) in dry ether (100 mL) was treated dropwise with a solution of ethanol (21.6 mL, 0.37 mol) and pyridine (29.6 mL, 0.37 mol) in ether (200 mL) at room tempeature under argon. After stirring for one hour, a mixture of water (6.6 mL, 0.37 mol) and pyridine (29.6 mL) was added slowly. The reaction mixture was filtered, washed with ether, and the ether evaporated to give an oil. The oil was distilled in the Kugelrohr and then through a short Vigreux column at 95°-98° C. (0.05 mmHg); lit. (T. L. Emmick et al., J. Am. Chem. Soc., 1968, 90, 3459) 102°-103° C. (0.2 mmHg). Yield 44.3 g (70%). 1H NMR (CDCl3)δ 7.57 (d, J=569 Hz, 1H), 8.0-7.4 (m, 5H), 4.13 (2 q, JH-H =7 Hz, JP-H =14 Hz, 2H), 1.35 (t, J=7 Hz, 3H).

후처리

  1. additionwas added slowly
  2. filtrationThe reaction mixture was filtered
  3. washwashed with ether
  4. customthe ether evaporated
  5. customto give an oil
  6. distillationThe oil was distilled in the Kugelrohr
  7. customat 95°-98° C.
  8. customlit. (T. L. Emmick et al., J. Am. Chem. Soc., 1968, 90, 3459) 102°-103° C. (0.2 mmHg)

출처 및 근거

ORD 기록
ord-16042fe0be94458d9afe54ff61d6b922
출처 데이터셋
uspto-grants-1986_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04574060

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