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Trimethyl borate → HCID 59713649、化合物

HRID 2223092
ノート
印刷プレビュー

反応式

HRID 2223092 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[N:3]=1.[Li]CCCC.B(OC)(OC)OC.Cl[C:23]1[C:29]2[CH:30]=[C:31]([Cl:34])[CH:32]=[CH:33][C:28]=2[N:27]([CH3:35])[C:26](=[O:36])[CH2:25][N:24]=1.[F-].[Cs+]>CCOCC.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.C(Cl)Cl.O.COCCOC>[Cl:34][C:31]1[CH:32]=[CH:33][C:28]2[N:27]([CH3:35])[C:26](=[O:36])[CH2:25][N:24]=[C:23]([C:2]3[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[N:3]=3)[C:29]=2[CH:30]=1
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

11

反応物 5

HCID 8470Trimethyl borateHCID 25953Cesium fluorideHCID 2568102-Bromo-6-methoxypyridineHCID 123385855,7-Dichloro-1-methyl-1,3-dihydro-2H-1,4-benzodiazepin-2-oneHCID 178418339Butyllithium

生成物 1

HCID 59713649HCID 59713649、化合物収率 57%

試薬・触媒・溶媒 5

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
-40 °C

実験手順

As illustrated in the scheme above, absolution of 2-bromo-6-methoxypyridine (0.022 mL, 0.18 mmol) in dry Et2O (0.3 mL) was added to a solution of n-BuLi (0.12 mL of 1.6 M in hexanes, 0.19 mmol) maintained at −40° C. The reaction was stirred at −40° C. for 20 min., and then B(OMe)3 (0.022 mL, 0.19 mmol) was added dropwise. The reaction was stirred at −40° C. for 30 min., and then at room temperature for 3.5 h. The reaction was concentrated in vacuo, anhydrous MeOH was added to the residue, and the reaction was concentrated in vacuo once again. Dry DME (0.8 mL), 5,7-dichloro-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (0.0392 g, 0.161 mmol), Pd(PPh3)4 (0.0093 g, 0.0080 mmol) and CsF (0.0612 g, 0.403 mmol) were added to the residue, and the mixture was heated to reflux for 15 h. Water (5 mL) and CH2Cl2 (5 mL) were added to the reaction mixture, and the layers were separated. The aqueous phase was extracted with additional CH2Cl2 (3×), and the combined organic phases were dried over Na2SO4, filtered, and concentrated in vacuo. Purification of the crude product by silica gel column chromatography (2:1 CH2Cl2:EtOAc) provided the title compound (0.029 g, 57%). 1H-NMR (CDCl3): δ 7.77 (d, J=7.6 Hz, 1H), 7.71-7.64 (m, 2H), 7.49 (dd, J=2.4 Hz, J=8.8 Hz, 1H), 7.27 (d, J=8.8 Hz, 1H), 6.83 (d, J=8.0 Hz, 1H), 4.85 (d, J=10.8 Hz, 1H), 3.86 (d, J=10.4 Hz, 1H), 3.81 (s, 3H), 3.39 (s, 3H). MS (ESI) (M+H)+=316.

後処理

  1. stirringThe reaction was stirred at −40° C. for 30 min.
  2. waitat room temperature for 3.5 h
  3. concentrationThe reaction was concentrated in vacuo, anhydrous MeOH
  4. additionwas added to the residue
  5. concentrationthe reaction was concentrated in vacuo once again
  6. temperaturethe mixture was heated
  7. temperatureto reflux for 15 h
  8. customthe layers were separated
  9. extractionThe aqueous phase was extracted with additional CH2Cl2 (3×)
  10. dry with materialthe combined organic phases were dried over Na2SO4
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo
  13. customPurification of the crude product by silica gel column chromatography (2:1 CH2Cl2:EtOAc)

出典と根拠

ORDレコード
ord-cc77d8070aac449f9b88e202867e4937
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07375101B2

反応ノート

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