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

HRID 1848904노트

반응식

HRID 1848904 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3475638025da444b886bf1f61ee746ce
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952157B2

반응 노트

불러오는 중…