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Hydrochloric Acid → HCID 22142147, 화합물

HRID 1824696
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HRID 1824696 반응식
Cl.[F:2][C:3]1[CH:4]=[C:5]([NH:20][NH2:21])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=1.N1C=CC=CC=1.[C:28](Cl)(=[O:30])[CH3:29].Cl>C(OCC)(=O)C.O>[F:2][C:3]1[CH:4]=[C:5]([NH:20][NH:21][C:28](=[O:30])[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 22142154HCID 22142154, 화합물

생성물 1

HCID 22142147HCID 22142147, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8857
Ethyl Acetate
용매

실험 절차

To [3-fluoro-4-[3-(trifluoromethyl)phenoxy]phenyl]hydrazine hydrochloride (0.35 g) prepared using the method described in Example 1, in ethyl acetate (5 mL), was added pyridine (0.24 mL) at −10° C. After dropwise addition of acetyl chloride (0.1 mL), the mixture was stirred for 3 h and then acidified with 6 M HCl. Water was added, and the product was extracted with ether. The organic layer was separated, dried, and concentrated. The residue was purified by column chromatography on silica (using dichloromethane, followed by 5:1 dichloromethane:ether as eluants) to give a solid (0.2 g).

후처리

  1. extractionthe product was extracted with ether
  2. customThe organic layer was separated
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica (using dichloromethane, followed by 5:1 dichloromethane:ether as eluants)

출처 및 근거

ORD 기록
ord-8d75ea7c051b451ca8495733475d3360
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07045512B2

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