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Hexane → N-tert-Butyl-2-chloro-5-[(E)-2-ethoxyvinyl]pyrimidin-4-amine

HRID 82167
ノート
印刷プレビュー

反応式

HRID 82167 の反応式
[B]1OC2C(=CC=CC=2)O1.[CH2:10]([O:12][C:13]#[CH:14])[CH3:11].CCCCCC.Br[C:22]1[C:23]([NH:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[N:24][C:25]([Cl:28])=[N:26][CH:27]=1.[OH-].[Na+]>C1COCC1.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.CCOC(C)=O>[C:30]([NH:29][C:23]1[C:22](/[CH:14]=[CH:13]/[O:12][CH2:10][CH3:11])=[CH:27][N:26]=[C:25]([Cl:28])[N:24]=1)([CH3:33])([CH3:31])[CH3:32]
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 8058HexaneHCID 14798Sodium HydroxideHCID 61239Ether, ethyl ethynylHCID 6327445BenzcatechinboraneHCID 790766715-Bromo-N-tert-butyl-2-chloropyrimidin-4-amine

生成物 1

HCID 86672092N-tert-Butyl-2-chloro-5-[(E)-2-ethoxyvinyl]pyrimidin-4-amine収率 55%

試薬・触媒・溶媒

3
HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

Catecholborane (7.8 g, 65.4 mmol) in THF (50 mL) was added dropwise to a solution of 40% ethoxyacetylene in hexane (12.8 mL, 72.5 mmol) under nitrogen at 0-5° C. The mixture was stirred for 2 hours at room temperature then heated at 70° C. for 2 hours. The mixture was then cooled to room temperature and a solution of 5-bromo-N-tert-butyl-2-chloropyrimidin-4-amine (10 g, 37.8 mmol) (see Preparation 60) in THF (50 mL) was added. The solution was degassed with argon for about 25 minutes followed by the addition of Pd(PPh3)4 (1.3 g, 1.13 mmol) and powdered sodium hydroxide (4.53 g, 113 mmol). The mixture was heated at 70° C. for 16 hours and then cooled to room temperature. EtOAc (200 mL) was added and the mixture was filtered through a Celite™ pad. The filtrate was evaporated in vacuo and the residue was purified by column chromatography on silica gel (gradient of hexane:EtOAc 93:7 to 90:10) to afford the title compound as a yellow oil in 55% yield, 5.3 g.

後処理

  1. temperaturethen heated at 70° C. for 2 hours
  2. temperatureThe mixture was then cooled to room temperature
  3. customThe solution was degassed with argon for about 25 minutes
  4. temperatureThe mixture was heated at 70° C. for 16 hours
  5. temperaturecooled to room temperature
  6. filtrationthe mixture was filtered through a Celite™ pad
  7. customThe filtrate was evaporated in vacuo
  8. customthe residue was purified by column chromatography on silica gel (gradient of hexane:EtOAc 93:7 to 90:10)

出典と根拠

ORDレコード
ord-4cf8f7e72045446fae6db9cdd0bd46ea
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

反応ノート

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