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Bromine → 5-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)phenoxy]-propyl]-2,5-dimethoxy-2,5-dihydrofuran

HRID 865694
ノート
印刷プレビュー

反応式

HRID 865694 の反応式
C(=O)([O-])[O-].[Na+].[CH3:6][C:7]1([O:32][CH3:33])[O:11][C:10]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[C:23]([CH3:24])=[CH:22][C:21]([C:25]3[N:26]=[N:27][N:28]([CH3:30])[N:29]=3)=[CH:20][C:19]=2[CH3:31])([O:12][CH3:13])[CH:9]=[CH:8]1.[Na+].CC1OC(CCCOC2C(C)=CC(C3N=NN(C)N=3)=CC=2C)=CC=1.BrBr>CO.[Cl-].[Na+].O>[CH3:6][C:7]1([O:32][CH3:33])[O:11][C:10]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[C:23]([CH3:24])=[CH:22][C:21]([C:25]3[N:26]=[N:27][N:28]([CH3:30])[N:29]=3)=[CH:20][C:19]=2[CH3:31])([O:12][CH3:13])[CH:9]=[CH:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24408BromineHCID 52730885-[3,5-Dimethyl-4-[3-(5-methyl-2-furyl)propoxy]phenyl]-2-methyl-tetrazoleHCID 677670605-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5 dimethoxy-2,5-dihydrofuran Sodium carbonate

生成物 1

HCID 229153545-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)phenoxy]-propyl]-2,5-dimethoxy-2,5-dihydrofuran収率 87%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
2 回
HCID 57417360Sodium chloride; water溶媒

実験手順

5-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5 dimethoxy-2,5-dihydrofuran Sodium carbonate (1.2 g) was added to a cooled (-10° C.) solution of 5-methyl 2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]furan from example 9d (780 mg, 2.4 mmol) in 18 mL of methanol with stirring, and then bromine (0.135 g, 14 mmol) in 8 mL of methanol was added dropwise until the brown color persisted, and the resulting reaction mixture was allowed to stir at -10° C. for 45 min. To the mixture was added brine, extracted with ether (3×25 mL), and the organic layer was washed with water, dried over magnesium sulfate, and concentrated in vacuo to yield an oil which was purified by MPLC chromatography (ethyl acetate/hexane 3:7) to afford 820 mg (76.3%) of 5-methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5-dimethoxy-2,5-dihyrofuran.

後処理

  1. customthe resulting reaction mixture
  2. stirringto stir at -10° C. for 45 min
  3. extractionextracted with ether (3×25 mL)
  4. washthe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto yield an oil which
  8. customwas purified by MPLC chromatography (ethyl acetate/hexane 3:7)

出典と根拠

ORDレコード
ord-59e3da985c9f435f8506b6e61a2150e6
出典データセット
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05567717

反応ノート

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