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

HRID 1043170ノート

反応式

HRID 1043170 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-893af5e6bc8146e78e88e578ec664467
出典データセット
uspto-grants-2013_10
特許番号
US08557983B2

反応ノート

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