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Potassium Phosphate, Tribasic → HCID 90409533、化合物

HRID 589036
ノート
印刷プレビュー

反応式

HRID 589036 の反応式
Br[C:2]1[C:11]2[O:10][CH2:9][CH:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:7]3[C:18](=[O:20])[NH:19][C:5]([C:6]=23)=[CH:4][CH:3]=1.[CH3:21][N:22]1[C:26](B2OC(C)(C)C(C)(C)O2)=[CH:25][CH:24]=[N:23]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCOCC1.O.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.NC1C=CC=CC=1C1C=CC=CC=1[Pd]Cl>[CH3:21][N:22]1[C:26]([C:2]2[C:11]3[O:10][CH2:9][CH:8]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)[N:7]4[C:18](=[O:20])[NH:19][C:5]([C:6]=34)=[CH:4][CH:3]=2)=[CH:25][CH:24]=[N:23]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

7

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 49129081-methyl-5-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 90409014HCID 90409014、化合物

生成物 1

HCID 90409533HCID 90409533、化合物収率 61.2%

試薬・触媒・溶媒 3

HCID 178439015HCID 178439015、化合物触媒
HCID 962
Water
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

7-Bromo-4-phenyl-4,5-dihydroimidazo[1,5,4-de][1,4]benzoxazin-2(1H)-one (100 mg, 0.3 mmol) was dissolved in 1,4-dioxane (2.4 mL). A solution of 1-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (94 mg, 0.45 mmol) and potassium phosphate (100 mg, 0.6 mmol) in water (0.60 mL) was added. Reaction was deoxygenated with nitrogen. Dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine-(2′-aminobiphenyl-2-yl)(chloro)palladium (1:1) (7 mg, 0.009 mmol) was added and deoxygenated with nitrogen. The reaction mixture was stirred at 100° C. for 4 h. Water and EtOAc were added and the layers were separated. The organic layer was concentrated under reduced pressure. Purification on silica using EtOAc/hexanes gave the title compound (61 mg). LCMS calc. for C19H17N4O2 (M+H)+: m/z=333.1. found: 333.2. 1H NMR (300 MHz, DMSO-d6): d 7.40 (s, 1H); 7.31 (m, 3H); 7.13 (m, 2H); 6.92 (m, 1H); 6.79 (m, 1H); 6.22 (s, 1H); 5.49 (s, 1H); 4.59 (m, 1H); 4.41 (m, 1H); 3.60 (s, 3H).

後処理

  1. customReaction
  2. customwas deoxygenated with nitrogen
  3. customdeoxygenated with nitrogen
  4. additionWater and EtOAc were added
  5. customthe layers were separated
  6. concentrationThe organic layer was concentrated under reduced pressure
  7. customPurification on silica

出典と根拠

ORDレコード
ord-47c5b7cd3f324dbfbc1bee6c49ba10c0
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09227985B2

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