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2-Bromopyrimidine → 3-[4-(2-Pyrimidinyl)phenyl]-2-propyn-1-ol

HRID 2416538
ノート
印刷プレビュー

反応式

HRID 2416538 の反応式
Br[C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)(O)[O-].[Na+].[OH:13][CH2:14][C:15]#[C:16][C:17]1[CH:22]=[CH:21][C:20](B(O)O)=[CH:19][CH:18]=1>COCCOC.O.C(Cl)Cl.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>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[C:20]1[CH:21]=[CH:22][C:17]([C:16]#[C:15][CH2:14][OH:13])=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 783452-BromopyrimidineHCID 516892Sodium BicarbonateHCID 22630943[4-(3-hydroxy-1-propynyl)phenyl]boronic Acid

生成物 1

HCID 226311353-[4-(2-Pyrimidinyl)phenyl]-2-propyn-1-ol収率 79%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A mixture of 2-bromopyrimidine (1.00 g, 6.29 mmol) and Pd(Ph3P)4 (220 mg, 0.19 mmol) in ethylene glycol dimethyl ether (25 mL) was stirred for 10 min, a slurry of sodium bicarbonate (1.58 g, 18.81 mmol) and [4-(3-hydroxy-1-propynyl)phenyl]boronic acid (1.32 g, 7.50 mmol, prepared as described in Reference Example 235) in water (25 mL) was added, and the mixture was heated to reflux for 4 h. The cooled reaction mixture was diluted with methylene chloride (100 mL) and washed with water (100 mL). The aqueous layer was extracted with dichloromethane (25 mL) and the combined organic layers were dried (MgSO4) and concentrated. Purification by chromatography (SiO2, 3:2 hexane/ethyl acetate) provided 1.04 g (79%) of the title compound as a yellow solid. MS 211 (M+H)+.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 h
  3. customThe cooled reaction mixture
  4. washwashed with water (100 mL)
  5. extractionThe aqueous layer was extracted with dichloromethane (25 mL)
  6. dry with materialthe combined organic layers were dried (MgSO4)
  7. concentrationconcentrated
  8. customPurification by chromatography (SiO2, 3:2 hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-98cbe00ca551436bb96fbe16248d5f21
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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