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Sodium Carbonate → HCID 178489480, 화합물

HRID 1170200
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HRID 1170200 반응식
[CH3:1][O:2][C:3]1[CH:22]=[CH:21][CH:20]=[CH:19][C:4]=1[CH2:5][NH:6][C:7]1[CH:16]=[CH:15][C:14]2[C:13]([C:17]#[N:18])=[CH:12][CH:11]=[CH:10][C:9]=2[N:8]=1.Cl.[NH2:24][OH:25].C(=O)([O-])[O-].[Na+].[Na+]>CCO.O>[OH:25][NH:24][C:17]([C:13]1[C:14]2[CH:15]=[CH:16][C:7]([NH:6][CH2:5][C:4]3[CH:19]=[CH:20][CH:21]=[CH:22][C:3]=3[O:2][CH3:1])=[N:8][C:9]=2[CH:10]=[CH:11][CH:12]=1)=[NH:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 67332820HCID 67332820, 화합물

생성물 1

HCID 178489480HCID 178489480, 화합물수율 90%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A stirred suspension of 2-(2-methoxy-benzylamino)-quinoline-5-carbonitrile (example 136, step B) (289 mg, 1.0 mmol), hydroxylamine hydrochloride (257 mg, 3.7 mmol) and sodium carbonate (212 mg, 2.0 mmol) in EtOH (4 ml) and water (4 ml) was heated under reflux conditions for 17 h, water (5 ml) was added, the precipitate was collected by filtration, washed with water and heptane and dried to yield the crude product as solid which was further purified by crystallization (diethyl ether/MeOH) to yield N-hydroxy-2-(2-methoxy-benzylamino)-quinoline-5-carboxamidine as off-white solid (290 mg, 90%).

후처리

  1. temperaturewas heated under reflux conditions for 17 h
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with water and heptane
  4. customdried
  5. customto yield the crude product as solid which
  6. customwas further purified by crystallization (diethyl ether/MeOH)

출처 및 근거

ORD 기록
ord-806924ca6c5b4285b521fcd84ed1d787
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07825253B2

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