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Benzaldehyde → HCID 58400975、化合物

HRID 1750904
ノート
印刷プレビュー

反応式

HRID 1750904 の反応式
Br[C:2]1[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[O:7][C:6]=2[CH:5]=[C:4](Br)[C:3]=1[NH2:16].[CH3:17][C:18]1(C)[C:22](C)(C)OB(C(C)=C)O1.[CH:29]1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)[CH2:34]CCC[CH2:30]1.C(=O)C1C=CC=CC=1.O.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>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].O.C1(C)C=CC=CC=1>[CH2:17]=[C:18]([C:2]1[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[O:7][C:6]=2[CH:5]=[C:4]([C:29]([CH3:34])=[CH2:30])[C:3]=1[NH2:16])[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 240BenzaldehydeHCID 109974264,4,5,5-Tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolaneHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 19737928HCID 19737928、化合物HCID 22031701Potassium phosphate, tribasic, monohydrate

生成物 1

HCID 58400975HCID 58400975、化合物

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

In a 3-neck, 500 mL round-bottom flask, 1,3-dibromodibenzo[b,d]furan-2-amine (19.24 g, 56.4 mmol), 4,4,5,5-tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane (30 g, 179 mmol), dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (1.85 g, 4.51 mmol), benzaldehyde (5.7 mL, 56.4 mmol), potassium phosphate monohydrate (52 g, 226 mmol), toluene (400 mL), and water (40 mL) were mixed. Nitrogen was bubbled directly into the mixture for 15 minutes, then Pd2(dba)3 (1.03 g, 1.13 mmol) was added. The reaction mixture was heated to reflux overnight. After cooled to room temperature, the organic layer was separated. 40 mL of concentrated HCl was added to the organic layer. The mixture was vigorously stirred for 1 h. Aqueous sodium hydroxide solution was added to basify the mixture. The organic layer was separated and purify by silica gel plug eluting with 1:1 dichloromethane/hexanes 19.1 g of a brown oil was obtained.

後処理

  1. customNitrogen was bubbled directly into the mixture for 15 minutes
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux overnight
  4. customthe organic layer was separated
  5. addition40 mL of concentrated HCl was added to the organic layer
  6. additionAqueous sodium hydroxide solution was added
  7. customThe organic layer was separated
  8. custompurify by silica gel plug
  9. washeluting with 1:1 dichloromethane/hexanes 19.1 g of a brown oil
  10. customwas obtained

出典と根拠

ORDレコード
ord-0c98d1f103504d839c1ea1c6b260fb5b
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156870B2

反応ノート

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