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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 57438892, 화합물

HRID 1669777
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HRID 1669777 반응식
N(OC(C)(C)C)=O.N[C:9]1[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]2[C:10]=1[C:11](=[O:21])[CH:12]=[C:13]([CH3:20])[O:14]2.[ClH:22]>C(#N)C.[Cu](Cl)Cl>[Cl:22][C:9]1[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]2[C:10]=1[C:11](=[O:21])[CH:12]=[C:13]([CH3:20])[O:14]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 10906Tert-Butyl nitriteHCID 57438891HCID 57438891, 화합물

생성물 1

HCID 57438892HCID 57438892, 화합물

시약·촉매·용매 2

HCID 24014Cupric Chloride촉매HCID 6342Acetonitrile용매2회

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온도
65 °C

실험 절차

0.42 g (3.9 mmol) of copper(II) chloride and 0.45 g (3.96 mmol) of tert-butyl nitrite are introduced into 20 ml of acetonitrile and heated to 65° C. 0.5 g (2.63 mmol) of 5-amino-2,8-dimethyl-4H-chromen-4-one in 10 ml of acetonitrile are slowly added dropwise to this suspension. The reaction mixture is stirred at 65° C. for 10 min and then allowed to cool to room temperature, and subsequently 5 ml of concentrated hydrochloric acid are added. After extraction with diethyl ether, the combined organic phases are washed with water and dried over sodium sulfate. After removal of the solvent in vacuo, the remaining crude product is purified by preparative HPLC. 0.27 g (50% of theory) of the title compound is obtained.

후처리

  1. temperatureto cool to room temperature
  2. extractionAfter extraction with diethyl ether
  3. washthe combined organic phases are washed with water
  4. dry with materialdried over sodium sulfate
  5. customAfter removal of the solvent in vacuo
  6. customthe remaining crude product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-59bc7e224068417b8013c1eb517ded98
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989633B2

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