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Ethanol → Ethyl 2-(tert-butoxy)-2-(3,5-diphenylthiophen-2-yl)acetate

HRID 590976
ノート
印刷プレビュー

反応式

HRID 590976 の反応式
[C:1]([O:5][CH:6]([C:12]1[S:13][C:14](Br)=[CH:15][C:16]=1Br)[C:7]([O:9][CH2:10][CH3:11])=[O:8])([CH3:4])([CH3:3])[CH3:2].[C:19]1(B(O)O)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:34](O)[CH3:35]>C1(C)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.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd].O>[C:1]([O:5][CH:6]([C:12]1[S:13][C:14]([C:35]2[CH:34]=[CH:16][CH:12]=[CH:6][CH:7]=2)=[CH:15][C:16]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])([CH3:4])([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 66827Phenylboronic AcidHCID 70819068Ethyl 2-(tert-butoxy)-2-(3,5-dibromothiophen-2-yl)acetate

生成物 1

HCID 70818072Ethyl 2-(tert-butoxy)-2-(3,5-diphenylthiophen-2-yl)acetate収率 51%

試薬・触媒・溶媒 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 962Water溶媒2 回
HCID 1140Toluene溶媒

反応条件

温度
95 °C

実験手順

A solution of ethyl 2-(tert-butoxy)-2-(3,5-dibromothiophen-2-yl)acetate (100 mg, 0.25 mmol), phenylboronic acid (36 mg, 0.30 mmol) and sodium carbonate (106 mg, 1.00 mmol) in a mixture of toluene (1.26 mL), ethanol (0.6 mL) and water (0.5 mL) was bubbled with nitrogen for 5 minutes. Palladium tetrakis(triphenylphosphine) (14 mg, 0.01 mmol) was added and the reaction mixture was heated a 95° C. overnight. After cooling to room temperature, water (2 mL) was added. The aqueous layer was extracted with toluene (2×8 mL). The organic layers were washed with brine (5 mL), dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (cyclohexane/ethyl acetate 80/20) to provide ethyl 2-(tert-butoxy)-2-(3,5-diphenylthiophen-2-yl)acetate (50 mg, 0.13 mmol, 51%).

後処理

  1. customwas bubbled with nitrogen for 5 minutes
  2. temperatureAfter cooling to room temperature
  3. extractionThe aqueous layer was extracted with toluene (2×8 mL)
  4. washThe organic layers were washed with brine (5 mL)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography on silica gel (cyclohexane/ethyl acetate 80/20)

出典と根拠

ORDレコード
ord-e1e5cb0b2cac407eaaddc8be046ea0a0
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238026B2

反応ノート

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