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Water → HCID 70818258, 화합물

HRID 591055
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HRID 591055 반응식
C(=O)([O-])[O-].[Na+].[Na+].O.I[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[C:15]([O:19][CH:20]([C:26]1[C:30](B2OC(C)(C)C(C)(C)O2)=[C:29]([CH3:40])[S:28][C:27]=1[CH3:41])[C:21]([O:23][CH2:24][CH3:25])=[O:22])([CH3:18])([CH3:17])[CH3:16]>CN(C)C=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd]>[C:15]([O:19][CH:20]([C:26]1[C:30]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:29]([CH3:40])[S:28][C:27]=1[CH3:41])[C:21]([O:23][CH2:24][CH3:25])=[O:22])([CH3:18])([CH3:17])[CH3:16]
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참가 물질

7

반응물 4

HCID 962Water2회HCID 10340Sodium CarbonateHCID 11575IodobenzeneHCID 70818507HCID 70818507, 화합물

생성물 1

HCID 70818258HCID 70818258, 화합물수율 75.6%

시약·촉매·용매 2

HCID 11979704
Tetrakis(triphenylphosphine)palladium
촉매
HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

Under argon atmosphere, sodium carbonate (18 mg, 0.169 mmol), water (1.1 mL) and iodobenzene (19 μL, 0.17 mmol) were added to a solution of ethyl 2-(tert-butoxy)-2-[2,5-dimethyl-4-(tetramethyl-1,3,2-dioxaborolan-2-yl)thiophen-3-yl]acetate (28f) (70 mg, 0.16 mmol) in N,N-dimethylformamide (3.4 mL). The solution was degassed under argon and palladium tetrakis(triphenylphosphine) (37 mg, 0.032 mmol) was added. The mixture was heated at 100° C. for 3 hours. The mixture was then cooled at room temperature, water was added and the aqueous layer was extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by preparative TLC (cyclohexane/ethyl acetate 90/10) to afford the desired product ethyl (28g) (42 mg, 0.121 mmol, 75%).

후처리

  1. customThe solution was degassed under argon
  2. temperatureThe mixture was then cooled at room temperature
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe residue was purified by preparative TLC (cyclohexane/ethyl acetate 90/10)

출처 및 근거

ORD 기록
ord-b0fb9884d5d946d3aa859016ef81b95e
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238026B2

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