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Potassium Carbonate → HCID 17756388, 화합물

HRID 491595
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HRID 491595 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][C:3]=1[O:4][CH2:5][C@@H:6]1[CH2:10][CH2:9][CH2:8][NH:7]1.Cl[Sn]Cl.[C:21]([O-])([O-])=O.[K+].[K+]>CCO>[Cl:1][C:2]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][C:3]=1[O:4][CH2:5][C@@H:6]1[CH2:10][CH2:9][CH2:8][N:7]1[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24479Stannous ChlorideHCID 17755967(S)-2-(2-Chloro-5-nitro-phenoxymethyl)-pyrrolidine

생성물 1

HCID 17756388HCID 17756388, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(S)-2-(2-Chloro-5-nitro-phenoxymethyl)-pyrrolidine (3.42 g, 12.63 mmol) and SnCl2 (7.19 g, 37.9 mmol) in 45 mL EtOH were heated at 75° C. for 11 h. The reaction was treated with about 15 mL 1 N K2CO3 (aq) and stirred 40 min. The suspension was filtered through Celite and concentrated down to aqueous, which was then diluted with EtOAc and 1 N NaOH (aq). The layers were separated, and the organic layer was washed twice with 1 N NaOH and once with mix of brine and 1 N NaOH. The aqueous layers were extracted twice with fresh EtOAc. The combined organic layers were dried over sodium sulfate, filtered, and concentrated down to dryness to yield the title compound as a brown solid.

후처리

  1. filtrationThe suspension was filtered through Celite
  2. concentrationconcentrated down to aqueous, which
  3. additionwas then diluted with EtOAc and 1 N NaOH (aq)
  4. customThe layers were separated
  5. washthe organic layer was washed twice with 1 N NaOH
  6. additiononce with mix of brine and 1 N NaOH
  7. extractionThe aqueous layers were extracted twice with fresh EtOAc
  8. dry with materialThe combined organic layers were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated down to dryness

출처 및 근거

ORD 기록
ord-d21d4a5b64d741e3bf38251270924748
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531553B2

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