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Triethylamine → HCID 86675814, 화합물

HRID 59877
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HRID 59877 반응식
[F:1][C:2]([F:30])([C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH:20]=[N:19][C:18]([C:21]3[CH:29]=[CH:28][C:24]([C:25]([OH:27])=O)=[CH:23][CH:22]=3)=[N:17]2)=[CH:12][CH:11]=1)[C:3]([F:9])([F:8])[C:4]([F:7])([F:6])[F:5].C1(P([N:45]=[N+:46]=[N-:47])(C2C=CC=CC=2)=O)C=CC=CC=1.C(N(CC)CC)C>C(O)(C)C>[F:1][C:2]([F:30])([C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH:20]=[N:19][C:18]([C:21]3[CH:29]=[CH:28][C:24]([C:25]([N:45]=[N+:46]=[N-:47])=[O:27])=[CH:23][CH:22]=3)=[N:17]2)=[CH:12][CH:11]=1)[C:3]([F:9])([F:8])[C:4]([F:6])([F:5])[F:7]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 866758154-(1-(4-(Perfluoropropyl)phenyl)-1H-1,2,4-triazol-3-yl)benzoic acid

생성물 1

HCID 86675814HCID 86675814, 화합물수율 30%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
0 °C

실험 절차

4-(1-(4-(Perfluoropropyl)phenyl)-1H-1,2,4-triazol-3-yl)benzoic acid (400 mg, 0.92 mmol) was dissolved in 7 mL of isopropanol and treated with diphenylphosphoryl azide (0.300 g, 1.09 mmol) and triethylamine (0.200 g, 2.0 mmol). The solution was allowed to stir for 6 h, then it was cooled to 0° C. and the resulting solid was filtered, washed with a minimum amount of iPrOH, and dried under high vacuum to give the azide as an off-white solid (0.120 g, 30%). This solid was not further characterized, but used directly in the subsequent Curtius rearrangement to prepare molecule A113, using conditions described in Example 39.

후처리

  1. filtrationthe resulting solid was filtered
  2. washwashed with a minimum amount of iPrOH
  3. customdried under high vacuum

출처 및 근거

ORD 기록
ord-a33441b0dd3944fda44ea0e5b23df0ef
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440964B2

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