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Hydrochloric Acid → 4-Fluoro-2-[(methylamino)carbonyl]benzylamine hydrochloride

HRID 2252802
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HRID 2252802 반응식
[ClH:1].[F:2][C:3]1[CH:17]=[CH:16][C:6]([CH2:7][NH:8]C(=O)OC(C)(C)C)=[C:5]([C:18]([NH:20][CH3:21])=[O:19])[CH:4]=1>C(OCC)(=O)C>[Cl-:1].[F:2][C:3]1[CH:17]=[CH:16][C:6]([CH2:7][NH3+:8])=[C:5]([C:18]([NH:20][CH3:21])=[O:19])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 11984298Tert-butyl 4-fluoro-2-[(methylamino)carbonyl]benzylcarbamate

생성물 1

HCID 866001764-Fluoro-2-[(methylamino)carbonyl]benzylamine hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Hydrogen chloride gas was bubbled through a −78° C. solution of tert-butyl 4-fluoro-2-[(methylamino)carbonyl]benzylcarbamate (615 mg, 2.18 mmol) in ethyl acetate (20 mL) until the solution was saturated. The flask was then allowed to warm to room temperature. The reaction was concentrated in vacud to a volume of about 5 mL and the flask was capped and placed in the freezer overnight. In the morning, the solids that had precipitated were collected by vacuum filtration and washed with cold ethyl acetate to give the desired product as an off-white solid.

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후처리

  1. concentrationThe reaction was concentrated in vacud to a volume of about 5 mL
  2. customthe flask was capped
  3. customplaced in the freezer overnight
  4. customIn the morning, the solids that had precipitated
  5. filtrationwere collected by vacuum filtration
  6. washwashed with cold ethyl acetate

출처 및 근거

ORD 기록
ord-354251217b304402ba879c1a01c4710c
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07323460B2

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