Sodium Hydroxide → 3-[1,1-bis(Methylethyl)-2-methyl-1-silapropoxy]phenol

HRID 985495노트

반응식

HRID 985495 반응식
[OH-].[Na+].C([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][Si:14]([CH:21]([CH3:23])[CH3:22])([CH:18]([CH3:20])[CH3:19])[CH:15]([CH3:17])[CH3:16])[CH:8]=1)(=O)C>C1COCC1>[CH3:20][CH:18]([Si:14]([CH:21]([CH3:23])[CH3:22])([O:13][C:9]1[CH:8]=[C:7]([OH:6])[CH:12]=[CH:11][CH:10]=1)[CH:15]([CH3:16])[CH3:17])[CH3:19]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 114610083-[1,1-bis(Methylethyl)-2-methyl-1-silapropoxy]phenyl acetate

생성물 1

HCID 225070633-[1,1-bis(Methylethyl)-2-methyl-1-silapropoxy]phenol수율 90.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

An aqueous (50 ml) solution of NaOH (3.25 g, 81 mmol) was added to a solution of 3-[1,1-bis(Methylethyl)-2-methyl-1-silapropoxy]phenyl acetate (5 g, 16.2 mmol) in THF (50 ml). After stirring overnight at room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried, filtered, and evaporated under vacuum. The crude product was chromatographed over silica gel to yield 3.89 g (90%) of 3-[1,1-bis(Methylethyl)-2-methyl-1-silapropoxy]phenol. NMR 1H Cl3CD δ: 7.06 (t, 1H, J=8.0 Hz), 6.42 (m, 3H), 1.28 (m, 3H), 1.10 (d, 18H, J=7.0 Hz).

후처리

  1. customthe reaction mixture was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated under vacuum
  6. customThe crude product was chromatographed over silica gel

출처 및 근거

ORD 기록
ord-4c6591ad39a34bf4a60003ffbef71e0a
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872730B2

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