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Sodium Carbonate → (2E)-3-[4-(5-bromo-2-pyrimidinyl)phenyl]-2-propen-1-ol

HRID 2416541
ノート
印刷プレビュー

反応式

HRID 2416541 の反応式
C([O-])([O-])=O.[Na+].[Na+].[Br:7][C:8]1[CH:9]=[N:10][C:11](I)=[N:12][CH:13]=1.[OH:15][CH2:16]/[CH:17]=[CH:18]/[C:19]1[CH:24]=[CH:23][C:22](B(O)O)=[CH:21][CH:20]=1>C1(C)C=CC=CC=1.C(OCC)(=O)C.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>[Br:7][C:8]1[CH:9]=[N:10][C:11]([C:22]2[CH:23]=[CH:24][C:19](/[CH:18]=[CH:17]/[CH2:16][OH:15])=[CH:20][CH:21]=2)=[N:12][CH:13]=1
参加物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 10340Sodium CarbonateHCID 70066515-Bromo-2-iodopyrimidineHCID 22630844[4-[(1E)-3-hydroxy-1-propenyl]phenyl]boronic Acid

生成物 1

HCID 22631131(2E)-3-[4-(5-bromo-2-pyrimidinyl)phenyl]-2-propen-1-ol収率 18%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 1140
Toluene
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

2 M aq. Na2CO3 (2 mL) was added to a mixture of 5-bromo-2-iodopyrimidine (0.57 g, 2.00 mmol), Pd(Ph3P)4 (23 mg, 0.020 mmol), and [4-[(1E)-3-hydroxy-1-propenyl]phenyl]boronic acid (360 mg, 2.02 mmol, prepared as described in Reference Example 238) in toluene (5 mL) and the resulting mixture was heated to reflux for 24 h. The cooled reaction mixture was diluted with ethyl acetate (20 mL) and the organic layer was separated, washed with brine (10 mL), dried (MgSO4) and concentrated. Purification by chromatography (SiO2, 3:1 hexane/ethyl acetate) provided 104 mg (18%) of the title compound as a yellow solid. MS 291, 293 (M+H)+.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux for 24 h
  3. customThe cooled reaction mixture
  4. customthe organic layer was separated
  5. washwashed with brine (10 mL)
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customPurification by chromatography (SiO2, 3:1 hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-0ad99f6dfe4145fb82c5805083372a9f
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06825170B2

反応ノート

読み込み中…

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