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Water → HCID 66939361, 화합물

HRID 1257422
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HRID 1257422 반응식
[OH:1][N:2]=[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[CH:6]=1)[NH2:4].Cl[C:16](=O)[CH2:17][N:18]1[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]1.O>N1C=CC=CC=1>[F:14][C:11]([F:13])([F:12])[C:7]1[CH:6]=[C:5]([C:3]2[N:4]=[C:16]([CH2:17][N:18]3[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]3)[O:1][N:2]=2)[CH:10]=[CH:9][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 609330N'-hydroxy-3-(trifluoromethyl)benzimidamideHCID 58127969HCID 58127969, 화합물

생성물 1

HCID 66939361HCID 66939361, 화합물수율 10.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
115 °C

실험 절차

A solution of N′-hydroxy-3-(trifluoromethyl)benzenecarboximidamide (2.1 g) in pyridine (20 mL) was cooled in an ice bath, and the compound (2.3 g) obtained in Example 115c was added. The reaction mixture was stirred overnight with heating at 110-120° C. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was separated, washed successively with 1N hydrochloric acid and saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.38 g) as a solid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe ethyl acetate layer was separated
  3. washwashed successively with 1N hydrochloric acid and saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)

출처 및 근거

ORD 기록
ord-bbb7264266f546f2b8552eebeb0808ec
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461348B2

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