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Chlorotrimethylsilane → [1-Hydroxy-4-methoxymethyl-6-(tetrahydro-pyran-2-yloxy)-1,3-dihydro-benzo[c][1,2]oxaborol-3-yl]-acetic acid ethyl ester

HRID 1798084
ノート
印刷プレビュー

反応式

HRID 1798084 の反応式
C[Si](Cl)(C)C.Br[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].[CH3:13][O:14][CH2:15][C:16]1[CH:23]=[C:22]([O:24][CH:25]2[CH2:30][CH2:29][CH2:28][CH2:27][O:26]2)[CH:21]=[C:20]([B:31]2[O:35][C:34](C)(C)C(C)(C)[O:32]2)[C:17]=1C=O>C1COCC1.[Zn]>[CH2:11]([O:10][C:8](=[O:9])[CH2:7][CH:34]1[O:35][B:31]([OH:32])[C:20]2[CH:21]=[C:22]([O:24][CH:25]3[CH2:30][CH2:29][CH2:28][CH2:27][O:26]3)[CH:23]=[C:16]([CH2:15][O:14][CH3:13])[C:17]1=2)[CH3:12]
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

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 7748Ethyl bromoacetateHCID 582928322-Methoxymethyl-4-(tetrahydro-pyran-2-yloxy)-6-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzaldehyde

生成物 1

HCID 58292743[1-Hydroxy-4-methoxymethyl-6-(tetrahydro-pyran-2-yloxy)-1,3-dihydro-benzo[c][1,2]oxaborol-3-yl]-acetic acid ethyl ester収率 67%

試薬・触媒・溶媒 2

HCID 23994
Zinc
触媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
55 °C

実験手順

A suspension of zinc (8.04 g, 123 mmol) in THF (80 mL) was added TMSCl (2.31 ml, 18.2 mmol) at 40° C. The temperature was increased to 55° C. over 30 min. Then, the temperature was lowered to 37° C. and ethyl 2-bromoacetate (12.6 mL, 114 mmol) was added slowly. The resulting solution was stirred for 30 min and cooled from 45° C. to room temperature and stood by for 1 h. The top clear layer (25 mL) was added to a solution of 2-methoxymethyl-4-(tetrahydro-pyran-2-yloxy)-6-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzaldehyde (3.56 g, 9.46 mmol) in THF (50 ml) at −78° C. After the addition, the reaction was warmed to 0° C. using an ice bath and stirred at 0° C. 30 min. The reaction mixture was quenched with aqueous NH4Cl and extracted with ethyl acetate. The organic phase was separated, dried (Na2SO4), and concentrated. The residue was purified by the flash column chromatography (silica, hexanes/ethyl acetate=2:1) to afford the title compound (2.30 g, 67%). 1H NMR (300 MHz, CDCl3) δ 7.33 (s, 1H), 7.11 (s, 1H), 5.73-5.70 (m, 1H), 5.46-5.44 (m, 1H), 4.54-4.39 (m, 2H), 4.21-4.16 (q, 2H), 3.94-3.90 (m, 1H), 3.66-3.60 (m, 1H), 3.38 (s, 3H), 3.18-3.11 (m, 1H), 2.43-2.34 (m, 1H), 1.88-1.85 (m, 2H), 1.70-1.61 (m, 4H), 1.26 (t, 3H).

後処理

  1. customwas lowered to 37° C.
  2. temperaturecooled from 45° C. to room temperature
  3. customstood by for 1 h
  4. additionAfter the addition
  5. temperaturethe reaction was warmed to 0° C.
  6. stirringstirred at 0° C
  7. custom30 min
  8. customThe reaction mixture was quenched with aqueous NH4Cl
  9. extractionextracted with ethyl acetate
  10. customThe organic phase was separated
  11. dry with materialdried (Na2SO4)
  12. concentrationconcentrated
  13. customThe residue was purified by the flash column chromatography (silica, hexanes/ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-c18f245b5b0c422e81fab59276f05d93
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08343944B2

反応ノート

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