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2-Chloro-6-fluorobenzaldehyde → [4-(5-Ethyl-3-pyridin-3-yl-pyrazol-1-yl)phenyl]-(2-chloro-6-fluorobenzyl)amine

HRID 1634118
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HRID 1634118 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH2:13][CH3:14])=[CH:11][C:10]([C:15]3[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=3)=[N:9]2)=[CH:4][CH:3]=1.[Cl:21][C:22]1[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[C:23]=1[CH:24]=O.C([BH3-])#N.[Na+]>CC(O)=O.CO>[CH2:13]([C:12]1[N:8]([C:5]2[CH:6]=[CH:7][C:2]([NH:1][CH2:24][C:23]3[C:26]([F:30])=[CH:27][CH:28]=[CH:29][C:22]=3[Cl:21])=[CH:3][CH:4]=2)[N:9]=[C:10]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)[CH:11]=1)[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 678472-Chloro-6-fluorobenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 186770941-(4-Aminophenyl)-3-(3-pyridyl)-5-ethylpyrazole

생성물 1

HCID 18677149[4-(5-Ethyl-3-pyridin-3-yl-pyrazol-1-yl)phenyl]-(2-chloro-6-fluorobenzyl)amine

시약·촉매·용매 1

HCID 10129899Acetic acid methanol용매

실험 절차

To a stirred solution of 1(4-aminophenyl)-3-(3-pyridyl)-5-ethylpyrazole (300 mg, 1.14 mmol) and 2-chloro-6-fluorobenzaldehyde (360 mg, 2.27 mmol) in 5% HOAc/MeOH (6 mL) at room temperature under argon was added sodium cyanoborohydride (180 mg, 2.86 mmol). The reaction mixture was stirred at room temperature for 4 h and then concentrated, diluted with water, extracted into ethyl acetate and washed with brine. The residue obtained on concentration was chromatographed on silica gel (eluant, gradient of 25-50% EtOAc in hexane) to provide the title compound as an oil which solidified on trituration with ether/petroleum (152 mg, 32%). m.p. 123-5° C. NMR (CDCl3, 400 MHz): 9.1 (s, 1H); 8.6 (br, 1H); 8.2 (br, 1H); 7.4-7.2 (overlapping m, 5H), 7.05 (m, 1H), 6.8 (d, 2H), 6.6 (s, 1H), 4.6 (s, 2H), 4.4 (br, 1H), 2.7 (q, 2H), 1.2 (t, 3H).

후처리

  1. concentrationconcentrated
  2. additiondiluted with water
  3. extractionextracted into ethyl acetate
  4. washwashed with brine
  5. customThe residue obtained on concentration
  6. customwas chromatographed on silica gel (eluant, gradient of 25-50% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-658c0f17102f496cb17bed5f437223b5
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06506747B1

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