Sodium hydride → Methyl 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyloxy)benzoate

HRID 1275610노트

반응식

HRID 1275610 반응식
[CH3:1][C:2]1([CH3:15])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([OH:14])[CH:5]=[CH:4][C:3]1=2.[H-].[Na+].I[C:19]1[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=1>[Cu](Br)Br.N1C=CC=CC=1>[CH3:1][C:2]1([CH3:15])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([O:14][C:19]3[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=3)[CH:5]=[CH:4][C:3]1=2

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 69273Methyl 4-iodobenzoateHCID 2687865,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol

생성물 1

HCID 10337221Methyl 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyloxy)benzoate

시약·촉매·용매 2

HCID 24611Copper bromide (CuBr2)촉매HCID 1049Pyridine용매

실험 절차

5.3 g (15 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol and 70 ml of pyridine were introduced into a three-necked flask under a nitrogen stream, and 430 mg (15 mmol) of sodium hydride (80% in oil) were added in small amounts. The mixture was stirred for 30 minutes, 3.9 g (15 mmol) of methyl 4-iodobenzoate and 4.6 g (22.5 mmol) of a copper bromide and dimethyl sulfide complex were added successively and the resulting mixture was heated at reflux for 16 hours. The reaction medium was evaporated to dryness, taken up in water and ethyl ether, the organic phase decanted off, dried over magnesium sulfate and evaporated.

후처리

  1. additionwere added in small amounts
  2. temperaturethe resulting mixture was heated
  3. temperatureat reflux for 16 hours
  4. customThe reaction medium was evaporated to dryness
  5. customethyl ether, the organic phase decanted off
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

출처 및 근거

ORD 기록
ord-2f3fa2a9de9e4c4081e8da7291a541f3
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162815

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