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1,2-Dimethoxyethane → HCID 68746268、化合物

HRID 1397482
ノート
印刷プレビュー

反応式

HRID 1397482 の反応式
[CH2:1]([N:3]1[CH2:8][CH2:7][C:6]([C:10]2[S:11][C:12](I)=[CH:13][N:14]=2)([OH:9])[CH2:5][CH2:4]1)[CH3:2].[C:16]([O:20][C:21]([NH:23][C:24]1[CH:29]=[CH:28][C:27](B(O)O)=[CH:26][C:25]=1[F:33])=[O:22])([CH3:19])([CH3:18])[CH3:17].[F-].[Cs+].C(COC)OC>C(OCC)(=O)C.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CO>[CH2:1]([N:3]1[CH2:8][CH2:7][C:6]([C:10]2[S:11][C:12]([C:27]3[CH:28]=[CH:29][C:24]([NH:23][C:21](=[O:22])[O:20][C:16]([CH3:17])([CH3:18])[CH3:19])=[C:25]([F:33])[CH:26]=3)=[CH:13][N:14]=2)([OH:9])[CH2:5][CH2:4]1)[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

9

反応物 4

HCID 80711,2-DimethoxyethaneHCID 25953Cesium fluorideHCID 222886774-N-Boc-Amino-3-fluorophenylboronic acidHCID 68720463HCID 68720463、化合物

生成物 1

HCID 68746268HCID 68746268、化合物

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物
触媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

A solution of Example 2A (0.33 g, 0.98 mmol), 4-(tert-butoxycarbonylamino)-3-fluorophenylboronic acid (0.25 g, 0.98 mmol), CsF (0.46 g, 3.0 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.12 g, 0.098 mmol) in a solvent mixture of dimethoxyethane (2 mL) and methanol (1 mL) was heated to 90° C. for 16 h. The reaction was cooled to ambient temperature and diluted with ethyl acetate (5 mL) and H2O (5 mL). The layers were separated, and the organic was washed with 10% aqueous HCl (3×15 mL). 2N NaOH was added to the combined acidic aqueous layers until pH=8. The aqueous layer was extracted with ethyl acetate (3×15 mL). The extracts were then dried with anhydrous Na2SO4, filtered, and concentrated under reduced pressure to give the title product as a solid. MS (ESI) m/z 422 [M+H]+.

後処理

  1. temperatureThe reaction was cooled to ambient temperature
  2. customThe layers were separated
  3. washthe organic was washed with 10% aqueous HCl (3×15 mL)
  4. addition2N NaOH was added to the combined acidic aqueous layers until pH=8
  5. extractionThe aqueous layer was extracted with ethyl acetate (3×15 mL)
  6. dry with materialThe extracts were then dried with anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c3ebab8761384134b03717c8581b458c
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901152B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート