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Phosgene → HCID 21072848, 화합물

HRID 1372900
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HRID 1372900 반응식
[C:1](Cl)(Cl)=[O:2].[NH2:5][C:6]1[CH:11]=CC=C[C:7]=1C(O)(C)C.N[CH2:17][C:18](C1C=CC=CC=1)=O.C[Mg]I.[CH2:29]1[CH2:33][O:32][CH2:31][CH2:30]1>>[CH3:7][C:6]1([CH3:11])[C:30]2[CH:29]=[CH:33][CH:17]=[CH:18][C:31]=2[O:32][C:1](=[O:2])[NH:5]1
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참가 물질

6

반응물 5

HCID 6371PhosgeneHCID 8028Tetrahydrofuran2회HCID 11952PhenacylamineHCID 2535272-(2-Aminophenyl)propan-2-olHCID 178418373HCID 178418373, 화합물

생성물 1

HCID 21072848HCID 21072848, 화합물

실험 절차

112 g (1.13 mol) phosgene are piped into 500 mL THF. Then a solution of 52 g (0.34 mol) 2-(2-amino-phenyl)-propan-2-ol, prepared from 2-aminoacetophenone and methylmagnesium iodide, in 300 mL THF is added. The reaction mixture is left to stand overnight, evaporated down and combined with 500 ml pyridine. After the pyridine has been distilled off water is added and the mixture is extracted with diethyl ether. The organic phases are washed successively with 2 N hydrochloric acid, sodium hydroxide solution and water, dried with sodium sulphate and evaporated down. The residue remaining (46 g) is further reacted directly without any more purification.

후처리

  1. additionis added
  2. waitThe reaction mixture is left
  3. customevaporated down
  4. distillationAfter the pyridine has been distilled off water
  5. additionis added
  6. extractionthe mixture is extracted with diethyl ether
  7. washThe organic phases are washed successively with 2 N hydrochloric acid, sodium hydroxide solution and water
  8. dry with materialdried with sodium sulphate
  9. customevaporated down
  10. customis further reacted directly without any more purification

출처 및 근거

ORD 기록
ord-dae4c0f8100449db99fdd854c66b7f30
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160882B2

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