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Hydrochloric Acid → 1-[(4,6-Di-t-butyl-5-hydroxy-2-methyl-2,3-dihydrobenzofuran-2-yl)methyl]thiourea

HRID 367310
ノート
印刷プレビュー

反応式

HRID 367310 の反応式
C([O:4][C:5]1[C:6]([C:24]([CH3:27])([CH3:26])[CH3:25])=[CH:7][C:8]2[O:12][C:11]([CH2:14][NH:15][C:16]([NH2:18])=[S:17])([CH3:13])[CH2:10][C:9]=2[C:19]=1[C:20]([CH3:23])([CH3:22])[CH3:21])(=O)C.[H-].C([Al+]CC(C)C)C(C)C.[Cl-].[NH4+].Cl>C1(C)C=CC=CC=1>[C:20]([C:19]1[C:9]2[CH2:10][C:11]([CH2:14][NH:15][C:16]([NH2:18])=[S:17])([CH3:13])[O:12][C:8]=2[CH:7]=[C:6]([C:24]([CH3:27])([CH3:26])[CH3:25])[C:5]=1[OH:4])([CH3:23])([CH3:21])[CH3:22]
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 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 21225700DiisobutylaluminumhydrideHCID 232880401-[(5-Acetoxy-4,6-di-t-butyl-2-methyl-2,3-dihydrobenzofuran-2-yl)methyl]thiourea

生成物 1

HCID 154857291-[(4,6-Di-t-butyl-5-hydroxy-2-methyl-2,3-dihydrobenzofuran-2-yl)methyl]thiourea収率 100%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Under a nitrogen atmosphere, 1.0 g of 1-[(5-acetoxy-4,6-di-t-butyl-2-methyl-2,3-dihydrobenzofuran-2-yl)methyl]thiourea was dissolved in 30 ml of toluene. To the solution was added 10.2 ml of diisobutyl aluminum hydride (1.0 M in toluene) and the mixture was stirred at room temperature for 1 hour. After reaction, the mixture was combined with a saturated aqueous ammonium chloride solution and 10% hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and then concentrated. The concentrate was purified by silica gel column chromatography eluting with n-hexane containing 33% ethyl acetate to give 0.89 g of 1-[(4,6-di-t-butyl-5-hydroxy-2-methyl-2,3-dihydrobenzofuran-2-yl)methyl]thiourea as a white crystal (yield 100%).

後処理

  1. customAfter reaction
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe concentrate was purified by silica gel column chromatography
  7. washeluting with n-hexane containing 33% ethyl acetate

出典と根拠

ORDレコード
ord-3e2c9dcfa8b84de39e383c05f0ed4b0e
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133279

反応ノート

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