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Boron tribromide → (4aR,6aR,11aR,11bR)-7,9-Dihydroxy-4,4,6a,11b-tetramethyl-1,2,4,4a,5,6,6a,11,11a,11b-decahydro-benzo[a]fluoren-3-one

HRID 1466729
ノート
印刷プレビュー

反応式

HRID 1466729 の反応式
C[O:2][C:3]1[CH:15]=[C:14]([O:16]C)[CH:13]=[C:12]2[C:4]=1[C@@:5]1([CH3:26])[C@H:10]([CH2:11]2)[C@@:9]2([CH3:25])[CH2:18][CH2:19][C:20](=[O:24])[C:21]([CH3:23])([CH3:22])[C@@H:8]2[CH2:7][CH2:6]1.B(Br)(Br)Br>C(Cl)Cl>[OH:2][C:3]1[CH:15]=[C:14]([OH:16])[CH:13]=[C:12]2[C:4]=1[C@@:5]1([CH3:26])[C@H:10]([CH2:11]2)[C@@:9]2([CH3:25])[CH2:18][CH2:19][C:20](=[O:24])[C:21]([CH3:22])([CH3:23])[C@@H:8]2[CH2:7][CH2:6]1
参加物反応条件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 25134Boron tribromideHCID 56837781(4aR,6aR,11aR,11bR)-7,9-Dimethoxy-4,4,6a,11b-tetramethyl-1,2,4,4a,5,6,6a,11,11a,11b-decahydro-benzo[a]fluoren-3-one2 回

生成物 1

HCID 56837782(4aR,6aR,11aR,11bR)-7,9-Dihydroxy-4,4,6a,11b-tetramethyl-1,2,4,4a,5,6,6a,11,11a,11b-decahydro-benzo[a]fluoren-3-one収率 86.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To ketone 6b (240 mg, 0.67 mmol) dissolved in 20 mL of methylene chloride stirring at 0° C. was added 2.7 mL of BBr3 (1.0 M in methylene chloride, 2.69 mmol). After stirring for one hour at 0° C., 6b was still present, and the reaction was allowed to reach room temperature over the next two hours. The reaction was then quenched with methanol, and water was added to the mixture. The aqueous phase was then extracted 3 times with methylene chloride (3×50 mL). The combined organic extracts were dried with MgSO4 and concentrated. The crude mixture was purified by flash chromatography to give 7b (190 mg, 0.578 mmol, 86%) as a white crystalline solid. 1H NMR (400 MHz, (CD3)2CO) δ 7.76 (s, 1H), 7.73 (s, 1H), 6.24 (t, J=0.96 Hz, 1H), 6.13 (d, J=1.6 Hz, 1H)), 2.66-2.61 (m, 1H), 2.59-2.52 (m, 2H), 2.49-2.46 (m, 1H), 2.44-2.37 (m, 1H), 1.86-1.82 (m, 1H), 1.81-1.77 (m, 1H), 1.76-1.71 (m, 1H), 1.67-1.55 (m, 4H), 1.15 (s, 3H), 1.13 (s, 3H), 1.07 (s, 3H), 1.09 (s, 3H); 13C NMR (100 MHz, (CD3)2CO) δ 216.9, 158.5, 154.8, 146.7, 131.9, 105.8, 102.8, 65.4, 57.2, 48.9, 47.3, 40.5, 39.6, 38.0, 35.4, 30.9, 27.9, 22.2, 22.1, 21.3, 16.9. ESIMS [M+Na]+ calcd for C21H28O3Na 351.1936, found 351.1929. [α]24D=+24.07°.

後処理

  1. customto reach room temperature over the next two hours
  2. customThe reaction was then quenched with methanol, and water
  3. additionwas added to the mixture
  4. extractionThe aqueous phase was then extracted 3 times with methylene chloride (3×50 mL)
  5. dry with materialThe combined organic extracts were dried with MgSO4
  6. concentrationconcentrated
  7. customThe crude mixture was purified by flash chromatography

出典と根拠

ORDレコード
ord-62963b6f9a9943e7b8cb73f1e16c0fef
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09000050B2

反応ノート

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