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Phosgene → HCID 21072848, 화합물

HRID 2223106
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HRID 2223106 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) of phosgene are piped into 500 mL of THF. Then a solution of 52 g (0.34 mol) of 2-(2-aminophenyl)propan-2-ol, prepared from 2-aminoacetophenone and methylmagnesium iodide, in 300 mL of THF is added. The reaction mixture is left to stand overnight, evaporated down, and combined with 500 mL of 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 sulfate, and evaporated down. The residue remaining (46 g) is further reacted directly without any more purification. M.p. (toluene/petroleum ether)=109° C.-110° C.

후처리

  1. additionis added
  2. waitThe reaction mixture is left
  3. customevaporated down
  4. distillationAfter the pyridine has been distilled off
  5. additionwater is 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 sulfate
  9. customevaporated down
  10. customis further reacted directly without any more purification

출처 및 근거

ORD 기록
ord-dbc33ff5a5b847719d94b7e23257ecec
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07375104B2

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