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Ethyl Acetate → HCID 117672588、化合物

HRID 712614
ノート
印刷プレビュー

反応式

HRID 712614 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([C:12]([NH2:14])=[O:13])[CH2:7][CH2:6][CH2:5]2.[C:15]([O:19][C:20](=[O:38])[NH:21][CH2:22][C:23]1[CH:24]=[N:25][CH:26]=[C:27](B2OC(C)(C)C(C)(C)O2)[CH:28]=1)([CH3:18])([CH3:17])[CH3:16].C([O-])([O-])=O.[Na+].[Na+].CCOC(C)=O>O1CCOCC1.O>[C:15]([O:19][C:20](=[O:38])[NH:21][CH2:22][C:23]1[CH:24]=[N:25][CH:26]=[C:27]([C:2]2[CH:11]=[N:10][C:9]3[N:8]([C:12](=[O:13])[NH2:14])[CH2:7][CH2:6][CH2:5][C:4]=3[CH:3]=2)[CH:28]=1)([CH3:18])([CH3:16])[CH3:17]
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

7

反応物 4

HCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 46739732tert-Butyl ((5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl)methyl)carbamateHCID 117667602HCID 117667602、化合物

生成物 1

HCID 117672588HCID 117672588、化合物収率 94.2%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

6-Bromo-3,4-dihydro-2H-[1,8]naphthyridine-1-carboxylic acid amide (79 mg, 0.31 mmol), [5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyridin-3-ylmethyl]-carbamic acid tert-butyl ester (205 mg, 0.61 mmol) and 2.0 M Na2CO3 aqueous solution (0.31 mL, 0.61 mmol) are dissolved in 2.0 mL of 1,4-dioxane. Argon gas is bubbled through the solution for 5 min. Then PdCl2dppf (16 mg, 0.021 mmol) is added. The mixture is heated at 100° C. for 2 hrs and the mixture is cooled down to room temperature. Then 30 mL of EtOAc and 20 mL of water are added and the organic layer is separated. The aqueous layer is extracted with EtOAc (2×20 mL). The organic layers are combined, dried and concentrated to give the crude product. Purification by flash column chromatography affords 112 mg of [5-(8-carbamoyl-5,6,7,8-tetrahydro-[1,8]naphthyridin-3-yl)-pyridin-3-ylmethyl]-carbamic acid tert-butyl ester

後処理

  1. customArgon gas is bubbled through the solution for 5 min
  2. temperaturethe mixture is cooled down to room temperature
  3. customthe organic layer is separated
  4. extractionThe aqueous layer is extracted with EtOAc (2×20 mL)
  5. customdried
  6. concentrationconcentrated
  7. customto give the crude product
  8. customPurification by flash column chromatography

出典と根拠

ORDレコード
ord-8d3649eda5974c089677693c91ea40f8
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181272B2

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