Triethylamine → HCID 86666324, 화합물

HRID 1026351노트

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HRID 1026351 반응식
[Br:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[CH2:9][C:10]([OH:12])=O.CN([C:16]([O:20][N:21]1N=NC2C=CC=N[C:22]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C.Cl.CNOC>ClCCl.O>[Br:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[CH2:9][C:10]([N:21]([O:20][CH3:16])[CH3:22])=[O:12]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 24721648(2-Bromo-4-hydroxyphenyl)acetic acid

생성물 1

HCID 86666324HCID 86666324, 화합물수율 97.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2-(2-bromo-4-hydroxyphenyl)acetic acid (0.67 g), HATU (1.33 g), triethylamine (0.35 g) and N,O-dimethylhydroxylamine hydrochloride (0.34 g) in dichloromethane (30 mL) was stirred overnight, to which water (30 mL) was added. The organic layer was separated. The water layer was extracted by ethyl acetate (20 mL×3). The combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to afford the title compound (773 mg).

후처리

  1. additionwas added
  2. customThe organic layer was separated
  3. extractionThe water layer was extracted by ethyl acetate (20 mL×3)
  4. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate)

출처 및 근거

ORD 기록
ord-f36d87ca33eb4713bd402beb990bfd1d
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729102B2

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