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Bicarbonate Ion → HCID 18455731、化合物

HRID 1272498
ノート
印刷プレビュー

反応式

HRID 1272498 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][N:6]([C:12](=[O:16])[CH2:13][CH2:14][OH:15])[C:5]2=[O:17].[Cl:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH3:26])[C:20]=1B(O)O.C(=O)([O-])[O-].[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)(O)[O-]>CN(C)C(=O)C.C(O)C.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(Cl)Cl>[Cl:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH3:26])[C:20]=1[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][N:6]([C:12](=[O:16])[CH2:13][CH2:14][OH:15])[C:5]2=[O:17]
参加物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 769Bicarbonate IonHCID 11430Potassium CarbonateHCID 11776TriphenylphosphineHCID 33782712-Chloro-6-methoxyphenylboronic acidHCID 18455748HCID 18455748、化合物

生成物 1

HCID 18455731HCID 18455731、化合物収率 24.3%

試薬・触媒・溶媒 5

HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒
HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 6-Bromo-3-(3-hydroxy-propionyl)-3H-quinazolin-4-one (11.6 mg, 0.039 mmol) dissolved in 1 ml N,N-dimethylacetamide in a 20 ml vial, 2-chloro-6-methoxy-phenylboronic acid (14.55 mg, 0.078 mmol) dissolved in 0.5 ml ethanol and potassium carbonate (5.92 mg, 0.043 mmol) dissolved in 0.5 ml water were added. Triphenylphosphine (1 mg, 3.8 umol) and tris(dibenzylideneacetone)dipalladium (0) (0.7 mg, 0.78 umol) were added to the mixture which refluxed overnight. The crude product was poured into 5 ml saturated bicarbonate solution and methylene chloride was used to extract the product. Solvent in the organic phase was removed under vacuum. The resulted residue was purified by preparative HPLC. 3.4 mg product was obtained. Yield: 24.3%; 1H NMR (500 MHz, DMSO-d6): δ 2.75538–2.78226(t, J=6.835 Hz, 2H), 3.70334(s, 3H), 4.15877–4.18594 (t, J=6.785 Hz, 2H), 7.13724–7.15535 (dd, J1=8.68 Hz, J2=0.75 Hz, 1H), 7.18337–7.20169 (dd, J1=8.375 Hz, J2=0.885 Hz, 1H), 7.41001–7.44275 (dd, J1=8.215 Hz, J2=8.185 Hz, 1H), 7.66453–7.68523 (dd, J1=8.38 Hz, J2=2.0 Hz, 1H), 7.72 (d, J=8.4 Hz, 1H), 7.96 (d, J=1.9 Hz, 1H), 8.41 (s, 1H); ESI-MS: m/z 359 (M++1)

後処理

  1. additionwere added
  2. temperaturerefluxed overnight
  3. extractionto extract the product
  4. customSolvent in the organic phase was removed under vacuum
  5. customThe resulted residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-7f11164dbc9448fca11e8636f69c4767
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07208493B2

反応ノート

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