Ammonium Chloride → HCID 11070377, 화합물

HRID 1452372노트

반응식

HRID 1452372 반응식
[Li].[C:2]([O:5][C:6]1[C:7]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:8][C:9]([OH:18])=[C:10]([C:13]=1[C:14]([CH3:17])([CH3:16])[CH3:15])[CH:11]=[O:12])(=[O:4])[CH3:3].Br[CH:24]([CH2:30][CH2:31][CH:32]([CH3:34])[CH3:33])[CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28].[Cl-].[NH4+]>O1CCCC1>[C:2]([O:5][C:6]1[C:7]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:8][C:9]([OH:18])=[C:10]([CH:11]([OH:12])[CH:24]([CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28])[CH2:30][CH2:31][CH:32]([CH3:33])[CH3:34])[C:13]=1[C:14]([CH3:15])([CH3:17])[CH3:16])(=[O:4])[CH3:3]

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 3028194LithiumHCID 110445455-Acetoxy-4,6-di-tert-butyl-2-hydroxybenzaldehydeHCID 22918674HCID 22918674, 화합물

생성물 1

HCID 11070377HCID 11070377, 화합물수율 46%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium (2.8 g) was added to a solution of 5-acetoxy-4,6-di-tert-butyl-2-hydroxybenzaldehyde (24.3 g) and 5-bromo-2,8-dimethylnonane (47.0 g) in tetrahydrofuran (200 ml) under ice cooling under a nitrogen atmosphere and the mixture was stirred overnight. The reaction mixture was poured into ice water, neutralized with a saturated aqueous solution of ammonium chloride and subjected to extraction with diethyl ether. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was distilled off. The residue was purified by silica gel chromatography (10% ethyl acetate in n-hexane) to afford 4-acetoxy-3,5-di-tert-butyl-2-(2,2-diisoamyl-1-hydroxyethyl)phenol [17.0 g (yield, 46%)] as a colorless oil.

후처리

  1. extractionsubjected to extraction with diethyl ether
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customThe residue was purified by silica gel chromatography (10% ethyl acetate in n-hexane)

출처 및 근거

ORD 기록
ord-6cf953d44fc64bf7804b90705ea53884
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606089

반응 노트

불러오는 중…