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Trimethyl borate → methyl hydrogen 5-methoxy-1-(triisopropylsilyl)-1H-pyrrolo[3,2-b]pyridin-6-ylboronate

HRID 2378971
ノート
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反応式

HRID 2378971 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]2[CH:9]=[CH:10][N:11]([Si:12]([CH:19]([CH3:21])[CH3:20])([CH:16]([CH3:18])[CH3:17])[CH:13]([CH3:15])[CH3:14])[C:6]2=[CH:5][CH:4]=1.[Li]CCCC.[B:27](OC)([O:30]C)[O:28][CH3:29]>C1COCC1>[CH3:1][O:2][C:3]1[N:8]=[C:7]2[CH:9]=[CH:10][N:11]([Si:12]([CH:16]([CH3:18])[CH3:17])([CH:13]([CH3:15])[CH3:14])[CH:19]([CH3:21])[CH3:20])[C:6]2=[CH:5][C:4]=1[B:27]([OH:30])[O:28][CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8470Trimethyl borateHCID 590063875-methoxy-1-(triisopropylsilyl)-1H-pyrrolo[3,2-b]pyridineHCID 178418339Butyllithium

生成物 1

HCID 59006331methyl hydrogen 5-methoxy-1-(triisopropylsilyl)-1H-pyrrolo[3,2-b]pyridin-6-ylboronate収率 42%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a colorless solution of 5-methoxy-1-(triisopropylsilyl)-1H-pyrrolo[3,2-b]pyridine (5.01 g, 16.45 mmol) in THF (100 mL) was dropwise added 2nd-BuLi (21.15 mL, 29.6 mmol) at −78° C. under N2 over 5 min to give an orange solution, the mixture was stirred for 30 min, followed by dropwise addition of trimethyl borate (3.31 mL, 29.6 mmol) through a syringe over 1 min. The resulting light orange solution was stirred at −78° C. for 1 hr, quenched with sat. NH4Cl (30 mL), partitioned between H2O/Et2O (100 mL/150 mL). After seperation, the organic layer was washed with brine (50 mL), dried on MgSO4, concentrated on rotary vacuo and purified on Biotage Flash Collector eluting with 10˜50% EtOAc/Hexanes (1300 mL) to afford the expected produce methyl hydrogen 5-methoxy-1-(triisopropylsilyl)-1H-pyrrolo[3,2-b]pyridin-6-ylboronate (2.5 g, 42%), as a colorless thick gum. Mass spec. 363.24 (MH+) calc. for C18H31,BN2O3 Si 362.22.

後処理

  1. customto give an orange solution
  2. stirringThe resulting light orange solution was stirred at −78° C. for 1 hr
  3. customquenched with sat. NH4Cl (30 mL)
  4. custompartitioned between H2O/Et2O (100 mL/150 mL)
  5. customAfter seperation
  6. washthe organic layer was washed with brine (50 mL)
  7. customdried on MgSO4
  8. concentrationconcentrated on rotary vacuo
  9. custompurified on Biotage Flash Collector
  10. washeluting with 10˜50% EtOAc/Hexanes (1300 mL)
  11. customto afford the

出典と根拠

ORDレコード
ord-9dec04fb0d274f2db7bb3bea8825a834
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07470680B2

反応ノート

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