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Triethylborane → Methyl (3R,5S,E)-7-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-3,5-dihydroxy-6-heptenoate

HRID 2050588
ノート
印刷プレビュー

反応式

HRID 2050588 の反応式
C(B(CC)CC)C.C(B(CC)OC)C.[F:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[N:23]=[C:24]([CH:46]([CH3:48])[CH3:47])[N:25](/[CH:34]=[CH:35]/[C@@H:36]([OH:45])[CH2:37][C:38](=[O:44])[CH2:39][C:40]([O:42][CH3:43])=[O:41])[C:26]=2[C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=2)=[CH:18][CH:17]=1.[BH4-].[Na+]>C(OCC)(=O)C.CO.C1COCC1>[F:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[N:23]=[C:24]([CH:46]([CH3:48])[CH3:47])[N:25](/[CH:34]=[CH:35]/[C@@H:36]([OH:45])[CH2:37][C@@H:38]([OH:44])[CH2:39][C:40]([O:42][CH3:43])=[O:41])[C:26]=2[C:27]2[CH:28]=[CH:29][C:30]([F:33])=[CH:31][CH:32]=2)=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7357TriethylboraneHCID 522516DiethylmethoxyboraneHCID 4311764Sodium borohydrideHCID 14849791methyl (5S,E)-7-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-5-hydroxy-3-oxo-6-heptenoate

生成物 1

HCID 14849841Methyl (3R,5S,E)-7-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-3,5-dihydroxy-6-heptenoate収率 48.7%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of dry THF (4 ml) and dry methanol (1 ml) under nitrogen at room temperature was treated with a solution of triethylborane (1.0M in THF, 0.6 ml). After 1 h, the mixture was cooled to -78°, and a portion of this diethyl methoxyborane solution (1.93 ml) was added to methyl (5S,E)-7-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-5-hydroxy-3-oxo-6-heptenoate (73.8 mg) under magnetic stirring. The homogeneous solution was stirred for 1 h, then treated with powdered sodium borohydride (98%, 6.4 mg) at -78°. After 4.5 h, the reaction mixture was diluted with ethyl acetate, quenched with saturated aqueous ammonium chloride solution and allowed to warm to room temperature overnight. The organic solution was separated and the aqueous solution washed with ether (3×). The combined organic solutions were dried and evaporated. The residue was azeotroped with methanol (3×) to give a brown gum. This gum was subjected to preparative t.l.c. eluting with System A (3:2), to give the title compound (36.1 mg) as a brown gum, [α]D20 +5.38° (c 1.86, ethyl acetate), δ(CDCl3) 1.40 (d, J 7 Hz, 6H, --CH(CH3)2), 1.4-1.8 (m, 2H, CH(OH)CH2CH(OH)), 2.44 (d, J 5 Hz, 2H, CH2CO2CH3), 3.13 (septet, J 7 Hz, 1H, --CH(CH3)2), 3.73 (s, 3H, OCH3), 3.85 (broad s, 2H, CH(OH)CH2CH(OH)), 4.15 (m, 1H, CH(OH)CH2CO2CH3), 4.42 (m, 1H, =CHCH(OH)CH2), 5.31 (dd, J 15 and 5 Hz, 1H, NCH=CH--), 6.66 (dd, J 15 and 2 Hz, 1H, NCH=CH--), 6.90 (t, J 9 Hz, 2H, C-3 and C-5 protons of 4-(4-fluorophenyl)), 7.09 (t, J 9 Hz, 2H, C-3 and C-5 protons of 5-(4-fluorophenyl)), 7.23 and 7.39 (2 dd, J 9 and 6 Hz, 4H, C-2 and C-6 protons of 4-fluorophenyls).

後処理

  1. temperaturethe mixture was cooled to -78°
  2. waitAfter 4.5 h
  3. customquenched with saturated aqueous ammonium chloride solution
  4. customThe organic solution was separated
  5. washthe aqueous solution washed with ether (3×)
  6. customThe combined organic solutions were dried
  7. customevaporated
  8. customThe residue was azeotroped with methanol (3×)
  9. customto give a brown gum
  10. washeluting with System A (3:2)

出典と根拠

ORDレコード
ord-895ac18065c24ee897eb093914224532
出典データセット
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05013749

反応ノート

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