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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 68408133, 화합물

HRID 505335
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HRID 505335 반응식
[NH2:1][C:2]1[C:13]([Cl:14])=[CH:12][CH:11]=[C:10]([Cl:15])[C:3]=1[C:4](N(OC)C)=[O:5].[CH2:16](OCC)C.Cl>C1COCC1.O>[NH2:1][C:2]1[C:13]([Cl:14])=[CH:12][CH:11]=[C:10]([Cl:15])[C:3]=1[C:4](=[O:5])[CH3:16]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 86608958HCID 86608958, 화합물

생성물 1

HCID 68408133HCID 68408133, 화합물수율 28%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

2-Amino-3,6-dichloro-N-methoxy-N-methyl-benzamide (2491 mg, 10 mmol) were dissolved in THF (100 ml). At −78° C. under nitrogen 1.6 M methyllithium solution in diethylether (25.0 ml, 40 mmol) were added dropwise and the reaction was allowed to reach room temperature and was stirred over night. The reaction was cooled in an icebath and 2N aqueous hydrogen chloride solution (30 ml) were added and the reaction was stirred for 30 min (r.t.). The reaction was diluted with water and extracted twice with diethyl ether. The combined organic layers were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and the solvent was evaporated. The residue was purified by column chromatography (CH2Cl2) to yield the product as an orange oil (565 mg, 28%).

후처리

  1. customto reach room temperature
  2. additionwere added
  3. stirringthe reaction was stirred for 30 min (r.t.)
  4. extractionextracted twice with diethyl ether
  5. washThe combined organic layers were washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. customThe residue was purified by column chromatography (CH2Cl2)

출처 및 근거

ORD 기록
ord-ef072b3d6e5d4885b5a1e158d746ad74
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781441B2

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