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Carbon tetrabromide → 6-(Bromomethyl)-2-methyl-1,3-benzoxazole

HRID 1888782
ノート
印刷プレビュー

反応式

HRID 1888782 の反応式
[CH3:1][C:2]1[O:3][C:4]2[CH:10]=[C:9]([CH2:11]O)[CH:8]=[CH:7][C:5]=2[N:6]=1.C(Br)(Br)(Br)[Br:14].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1>[Br:14][CH2:11][C:9]1[CH:8]=[CH:7][C:5]2[N:6]=[C:2]([CH3:1])[O:3][C:4]=2[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 15662270(2-Methylbenzo[d]oxazol-6-yl)methanol

生成物 1

HCID 670157966-(Bromomethyl)-2-methyl-1,3-benzoxazole

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of (2-methyl-1,3-benzoxazol-6-yl)methanol (66.5 mg, 0.408 mmol) in toluene (1 mL) were added carbon tetrabromide (135 mg, 0.408 mmol) and triphenylphosphine (106 mg, 0.408 mmol) and the mixture was stirred at room temperature for 30 min. The reaction mixture was directly applied to silica gel, and concentrated to dryness to give 6-(bromomethyl)-2-methyl-1,3-benzoxazole as an oil. To the obtained oil (92.0 mg, 0.408 mmol) were added DMF (4 mL), N-[1-(5-hydroxy-1-benzofuran-2-yl)ethyl]acetamide (30.0 mg, 0.136 mmol) obtained in Reference Example 38 and potassium carbonate (37.8 mg, 0.274 mmol), and the mixture was stirred at 50° C. for 2 hr. The reaction mixture was directly purified by basic silica gel column chromatography (hexane:ethyl acetate-4:1 to 3:7), and the solvent was evaporated. The residue was triturated with a small amount of ethyl acetate and diethyl ether to give the title compound (17.8 mg, yield 36%) as a white solid.

後処理

  1. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-241508f24f9f4b3eba7205dca8a5f63e
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501804B2

反応ノート

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