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Sodium Methoxide → 1-Bromo-2,3-dichloro-5-methoxybenzene

HRID 339642
ノート
印刷プレビュー

反応式

HRID 339642 の反応式
[Br:1][C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4]([Cl:9])[C:3]=1[Cl:10].[CH3:11][O-:12].[Na+]>C1COCC1>[Br:1][C:2]1[CH:7]=[C:6]([O:12][CH3:11])[CH:5]=[C:4]([Cl:9])[C:3]=1[Cl:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 216910511-Bromo-2,3-dichloro-5-fluorobenzene

生成物 1

HCID 577991521-Bromo-2,3-dichloro-5-methoxybenzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-Bromo-2,3-dichloro-5-fluorobenzene (5.1453 g, 21.10 mmol) was dissolved in THF (25 mL) at room temperature and cooled to 0° C. Then, 5.1 g of sodium hydride (60%, 128 mmol) was added and 2.0 mL of methanol was added slowly. Additional THF (5 mL) was added. The mixture was stirred at room temperature for 10 minutes, then heated at 75° C. for four hours and cooled to room temperature. The mixture was poured into ice with some aq. sat. NH4Cl solution and extracted with EtOAc (3×100 mL). The organic solution was washed with brine, dried over Na2SO4, concentrated to dryness. The residue was purified with flash column chromatography on silica gel using hexane as solvent to afford the product (4.6727 g) as a white solid in 87% yield. 1H-NMR (CDCl3): δ 7.109 (d, J=3.0 Hz, 1H), 6.988 (d, J=3.0 Hz, 1H), 3.786 (s, 3H). The product was also synthesized from 1-bromo-2,3-dichloro-5-fluorobenzene and sodium methoxide in THF. The final product was purified by recrystallization from hexane.

後処理

  1. customThe final product was purified by recrystallization from hexane

出典と根拠

ORDレコード
ord-e75c161c54f9448eae2219a90ad4336c
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895553B2

反応ノート

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