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O-Phenylenediamine → HCID 136352247, 화합물

HRID 1047531
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HRID 1047531 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[N:7]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=3)=[CH:13][CH:14]=2)[C:9]([CH:26]=O)=[N:8]1.[C:28]1([NH2:35])[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[NH2:34].S(=O)(O)[O-].[Na+]>C1COCC1.Cl.C(OCC)(=O)C>[NH:34]1[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=2[N:35]=[C:26]1[C:9]1[C:10]2[C:15](=[CH:14][CH:13]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=3)[CH:11]=2)[N:7]([CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][O:1]2)[N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 7243O-PhenylenediamineHCID 23665763Sodium BisulfiteHCID 86673212HCID 86673212, 화합물

생성물 1

HCID 136352247HCID 136352247, 화합물수율 50%

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

1-(Tetrahydro-2H-pyran-2-yl)-5-(3-(trifluoromethyl)phenyl)-1H-indazole-3-carbaldehyde (15 mg, 0.040 mmol) and o-phenylene diamine (5 mg, 0.046 mmol) were dissolved in dry THF (5 mL) and 2N HCl (1 drop) was added. The solution was heated at a gentle reflux for 30 min and then 1N sodium bisulfite (1 mL) was added. After overnight at reflux, the solution was cooled to room temperature, and diluted with ethyl acetate (25 mL). The mixture was washed with water and brine, dried over Na2SO4, and concentrated. Purification by flash chromatography (20% ethyl acetate/hexane) afforded the title compound as a pale yellow solid in a 50% yield. 1H NMR (400 MHz, CD3OD): δ 9.91 (s, 1H), 8.81 (s, 1H), 7.89-7.82 (m, 2H), 7.66 (m, 2H), 7.55-7.44 (m, 3H), 7.24 (m, 2H), 5.77 (dd, 1H, J=2.4 and 9.2 Hz), 4.02 (m, 1H), 3.75 (m, 1H), 2.59 (m, 1H), 2.12 (m, 2H), 1.75 (m, 3H); ESI-MS [M+H]+: 463.3.

후처리

  1. temperatureThe solution was heated at
  2. temperaturea gentle reflux for 30 min
  3. temperatureAfter overnight at reflux
  4. washThe mixture was washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customPurification by flash chromatography (20% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-75bcf632fa5542d583b6bed9823a249a
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569511B2

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