Ammonium tetrafluoride → 1-(4-methoxybenzyl)-1H-1,2,3-benzotriazol-4-ol

HRID 624425ノート

反応式

HRID 624425 の反応式
C([Si](C)(C)[O:6][C:7]1[C:15]2[N:14]=[N:13][N:12]([CH2:16][C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)[C:11]=2[CH:10]=[CH:9][CH:8]=1)(C)(C)C.[F-].[NH4+].[NH4+].[NH4+].[NH4+].[F-].[F-].[F-]>O1CCCC1>[CH3:24][O:23][C:20]1[CH:19]=[CH:18][C:17]([CH2:16][N:12]2[C:11]3[CH:10]=[CH:9][CH:8]=[C:7]([OH:6])[C:15]=3[N:14]=[N:13]2)=[CH:22][CH:21]=1

参加物

4

反応物 2

HCID 22393694Ammonium tetrafluorideHCID 672271234-(Tert-butyl-dimethyl-silanyloxy)-1-(4-methoxy-benzyl)-1h-benzotriazole

生成物 1

HCID 1363439141-(4-methoxybenzyl)-1H-1,2,3-benzotriazol-4-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of EXAMPLE 342B (2.59 g) in tetrahydrofuran (40 mL) was added tetraammonium fluoride (1M in tetrahydrofuran, 21.03 mL). The solution was mixed at room temperature for two hours. The solvent was removed under vacuum, the residue was taken up in ethyl acetate, and the solution was vacuum filtered over a pad of silica gel. The filtrate was concentrated and purified by flash column chromatography on silica gel using 35% ethyl acetate in hexanes.

後処理

  1. additionThe solution was mixed at room temperature for two hours
  2. customThe solvent was removed under vacuum
  3. filtrationfiltered over a pad of silica gel
  4. concentrationThe filtrate was concentrated
  5. custompurified by flash column chromatography on silica gel using 35% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-f7caf6fa51384d43a873764f003672ce
出典データセット
uspto-grants-2016_04
特許番号
US09303025B2

反応ノート

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