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Lithium Hexamethyldisilazide → HCID 86700871、化合物

HRID 881762
ノート
印刷プレビュー

反応式

HRID 881762 の反応式
[Cl-].[CH3:2][O:3][CH3:4].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[CH:34]1([C:38]2[O:42][C:41]([NH:43][C:44]3[CH:45]=[CH:46][C:47]([C:50]4[CH:55]=[CH:54][C:53]([C:56]56[CH2:63][CH2:62][C:59]([CH:64]=O)([CH2:60][CH2:61]5)[CH2:58][O:57]6)=[CH:52][CH:51]=4)=[N:48][CH:49]=3)=[N:40][N:39]=2)[CH2:37][CH2:36][CH2:35]1>O1CCCC1>[CH:34]1([C:38]2[O:42][C:41]([NH:43][C:44]3[CH:49]=[N:48][C:47]([C:50]4[CH:55]=[CH:54][C:53]([C:56]56[CH2:63][CH2:62][C:59]([CH:64]=[CH:2][O:3][CH3:4])([CH2:60][CH2:61]5)[CH2:58][O:57]6)=[CH:52][CH:51]=4)=[CH:46][CH:45]=3)=[N:40][N:39]=2)[CH2:35][CH2:36][CH2:37]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

5

反応物 3

HCID 2733832Lithium HexamethyldisilazideHCID 86700853HCID 86700853、化合物HCID 89872208HCID 89872208、化合物

生成物 1

HCID 86700871HCID 86700871、化合物収率 31.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a stirred suspension of triphenylphosphine methoxymethane chloride (28.7 mg, 0.084 mmol) in tetahydrofuran (1 ml) was flushed with nitrogen for three times and at 0° C., and was added LiHMDS (0.079 ml, 0.084 mmol). The reddish solution was stirred at 0° C. for 30 minutes, and then at −78° C., a solution of 1-(4-(5-((5-cyclobutyl-1,3,4-oxadiazol-2-yl)amino)pyridin-2-yl)phenyl)-2-oxabicyclo[2.2.2]octane-4-carbaldehyde (30 mg, 0.070 mmol) in tetrahydrofuran (0.7 ml) was added dropwise. The mixture was allowed to warm to 0° C. for 30 minutes. The reaction was quenched with water (2 ml), and the mixture was partitioned between brine (15 ml) and ethyl acetate (50 ml), aquous layer was extracted with ethyl acetate (2×50 ml). The combined organic extracts were washed with brine and dried over Na2SO4, and concentrated. The residue was purified by flash chromatography (heptanes/acetone 1/1) to afford 5-cyclobutyl-N-(6-(4-(4-(2-methoxyvinyl)-2-oxabicyclo[2.2.2]octan-1-yl)phenyl)pyridin-3-yl)-1,3,4-oxadiazol-2-amine (10 mg, 31%) as yellow solid. 1H NMR (400 MHz, METHANOL-d4) δ ppm 1.83-2.51 (m, 14H) 3.56 (s, 3H) 3.63-3.76 (m, 1H) 4.00 (d, J=6.80 Hz, 1H) 4.06 (s, 2H) 5.87 (d, J=6.80 Hz, 1H) 7.49 (d, J=8.72 Hz, 2H) 7.78-7.93 (m, 3H) 8.17 (dd, J=24.00, 8.80 Hz, 1H) 8.71 (d, J=16.80 Hz, 1H). LC/MS, [MS+1] 459.1, RT: 1.44, 1.48; (Condition E).

後処理

  1. customwas flushed with nitrogen for three times and at 0° C.
  2. temperatureto warm to 0° C. for 30 minutes
  3. customThe reaction was quenched with water (2 ml)
  4. customthe mixture was partitioned between brine (15 ml) and ethyl acetate (50 ml), aquous layer
  5. extractionwas extracted with ethyl acetate (2×50 ml)
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography (heptanes/acetone 1/1)

出典と根拠

ORDレコード
ord-0e9595dd09ac4da6b64f857b01f5ea70
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993619B2

反応ノート

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