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Potassium Carbonate → HCID 86600751、化合物

HRID 2252456
ノート
印刷プレビュー

反応式

HRID 2252456 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C@H:11]([C:12]3[CH:17]=[CH:16][C:15](B4OC(C)(C)C(C)(C)O4)=[CH:14][CH:13]=3)[C@@H:10]([CH2:27][CH2:28][C@@H:29]([C:31]3[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=3)[OH:30])[C:9]2=[O:38])=[CH:4][CH:3]=1.[CH2:39]([O:46][C@@H:47]1[C@@H:54]([O:55][CH2:56][C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=2)[C@H:53]([O:63][CH2:64][C:65]2[CH:70]=[CH:69][CH:68]=[CH:67][CH:66]=2)[C@@H:52]([CH2:71][O:72][C:73]2[CH:78]=[CH:77][CH:76]=[C:75](Br)[CH:74]=2)[O:51][CH:48]1[O:49][CH3:50])[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C(CCO)=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:39]([O:46][C@@H:47]1[C@@H:54]([O:55][CH2:56][C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=2)[C@H:53]([O:63][CH2:64][C:65]2[CH:70]=[CH:69][CH:68]=[CH:67][CH:66]=2)[C@@H:52]([CH2:71][O:72][C:73]2[CH:74]=[C:75]([C:15]3[CH:14]=[CH:13][C:12]([C@@H:11]4[C@@H:10]([CH2:27][CH2:28][C@@H:29]([C:31]5[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=5)[OH:30])[C:9](=[O:38])[N:8]4[C:5]4[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=4)=[CH:17][CH:16]=3)[CH:76]=[CH:77][CH:78]=2)[O:51][C@@H:48]1[O:49][CH3:50])[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=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

6

反応物 3

HCID 11430Potassium CarbonateHCID 69125242HCID 69125242、化合物HCID 69125699HCID 69125699、化合物

生成物 1

HCID 86600751HCID 86600751、化合物収率 85%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 88267
2-Methylphenethyl alcohol
溶媒

反応条件

温度
85 °C

実験手順

(3R,4S)-1-(4-Fluorophenyl)-3-[(3S)-3-(4-fluorophenyl)-3-hydroxypropyl]-4-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]azetidin-2-one (64.1 mg, 0.12 mmol), methyl 2,3,4-tri-O-benzyl-6-O-(3-bromophenyl)-D-glucopyranoside (54.6 mg, 0.09 mmol), and potassium carbonate (88 μL, 2 M aqueous solution) were dissolved in 1:1 toluen-ethanol (1 mL total volume). The solution was degassed by evacuating the vessel and flushing with argon three times. Tetrakis(triphenylphosphine)palladium (5.1 mg, 0.004 mmol) was added and the solution degassed twice. The reaction was heated at 85° C. for 1 h. LCMS and TLC (1:1 hexane-ethyl acetate) analysis indicated consumption of the starting glycoside. The reaction was diluted into ethyl acetate (30 mL) and washed with water (2×10 mL). The combined aqueous washes were back extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous sodium sulfate, filtered, concentrated in vacuo and purified by chromatography (12 g silica gel, 20% to 50% ethyl acetate-hexane) to afford methyl 2,3,4-tri-O-benzyl-6-O-(4′-{(2S,3R)-1-(4-fluorophenyl)-3-[(3S)-3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}biphenyl-3-yl)-α-D-glucopyranoside (70.0 mg, 85% yield). 1H NMR (300 MHz, CDCl3) δ 7.55 (d, J=8.1 Hz, 2H), 7.39-6.84 (m, 29H), 5.01 (d, J=10.8 Hz, 1H), 4.89-4.80 (m, 3H), 4.73-4.64 (m, 4H), 4.52 (d, J=11.1 Hz, 1H), 4.15-4.12 (m, 2H), 4.08-4.-1 (m, 1H), 3.94-3.90 (m, 1H), 3.77-3.71 (m, 1H), 3.62 (dd, J=3.6 Hz, J=9.6 Hz, 1H), 3.39 (s, 3H), 3.13-3.10 (m, 1H), 2.03-1.89 (m, 4H) ppm.

後処理

  1. customThe solution was degassed
  2. customby evacuating the vessel
  3. customflushing with argon three times
  4. customthe solution degassed twice
  5. customconsumption of the starting glycoside
  6. additionThe reaction was diluted into ethyl acetate (30 mL)
  7. washwashed with water (2×10 mL)
  8. extractionThe combined aqueous washes were back extracted with ethyl acetate (2×10 mL)
  9. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo
  12. custompurified by chromatography (12 g silica gel, 20% to 50% ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-c3ac0c6435614a9ab82bd00468a62db8
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07320972B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート