Potassium Carbonate → 5-Bromo-2-[(3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)acetyl]thiophene

HRID 1075630노트

반응식

HRID 1075630 반응식
[I:1][C:2]1[C:3]([OH:16])=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.Br[CH2:18][C:19]([C:21]1[S:22][C:23]([Br:26])=[CH:24][CH:25]=1)=[O:20].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C>[Br:26][C:23]1[S:22][C:21]([C:19](=[O:20])[CH2:18][O:16][C:3]2[C:2]([I:1])=[CH:11][C:10]3[C:9]([CH3:12])([CH3:13])[CH2:8][CH2:7][C:6]([CH3:15])([CH3:14])[C:5]=3[CH:4]=2)=[CH:25][CH:24]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 19883982-Bromo-1-(5-bromothiophen-2-yl)ethan-1-oneHCID 107114633-Iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol

생성물 1

HCID 701951435-Bromo-2-[(3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)acetyl]thiophene

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A solution of 3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol (4 g, 12.1 mmol), 2-bromoacetyl-5-bromothiophene (3.44 g, 12.1 mmol) and potassium carbonate (1.8 g, 13.3 mmol) in methyl ethyl ketone (100 ml), was heated under reflux for 3 h. The reaction medium was filtered and then concentrated in a rotary evaporator, and water and ethyl ether were added. After stirring and decantation, the organic phase was washed twice with water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C.

후처리

  1. temperatureunder reflux for 3 h
  2. filtrationThe reaction medium was filtered
  3. concentrationconcentrated in a rotary evaporator, and water and ethyl ether
  4. additionwere added
  5. washdecantation, the organic phase was washed twice with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in a rotary evaporator under vacuum at 40° C.

출처 및 근거

ORD 기록
ord-5f19d11b409247419627fa73c80882d7
출처 데이터셋
uspto-grants-1999_05
특허 번호
US05905088

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