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Lithium diisopropylamide → HCID 90372982、化合物

HRID 930365
ノート
印刷プレビュー

反応式

HRID 930365 の反応式
C([N-]C(C)C)(C)C.[Li+].O1CCCC1.CCCCCCC.C(C1C=CC=CC=1)C.[CH3:29][N:30]([CH3:38])/[N:31]=[C:32](\[CH3:37])/[C:33]([F:36])([F:35])[F:34].[Br:39][C:40]1[CH:41]=[C:42](/[C:47](=[N:50]\[S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])/[CH2:48][F:49])[C:43]([F:46])=[N:44][CH:45]=1>C1COCC1.C1(C)C=CC=CC=1>[Br:39][C:40]1[CH:41]=[C:42]([C@@:47]([NH:50][S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])([CH2:37]/[C:32](=[N:31]/[N:30]([CH3:38])[CH3:29])/[C:33]([F:36])([F:35])[F:34])[CH2:48][F:49])[C:43]([F:46])=[N:44][CH:45]=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

7

反応物 4

HCID 2724682Lithium diisopropylamideHCID 22742125Tetrahydrofuran heptane ethylbenzolHCID 58668234HCID 58668234、化合物HCID 90373167HCID 90373167、化合物

生成物 1

HCID 90372982HCID 90372982、化合物収率 68.8%

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

Lithium diisopropylamide, 2.0M solution in tetrahydrofuran/heptane/ethylbenzene (1.474 ml, 2.95 mmol) was added dropwise via syringe to a solution of (E)-1,1-dimethyl-2-(1,1,1-trifluoropropan-2-ylidene)hydrazine (0.454 g, 2.95 mmol) in THF 4.0 mL at −78° C. After stirring at −78° C. for 1 h, the solution was added dropwise via cannula to a solution of (R,E)-N-(1-(5-bromo-2-fluoropyridin-3-yl)-2-fluoroethylidene)-2-methylpropane-2-sulfinamide (0.500 g, 1.474 mmol) in toluene 4 mL cooled to −78° C. The reaction was stirred 3 h at −78° C. before being quenched with saturated aqueous ammonium chloride at −78° C. The mixture was warmed up to room temperature and diluted with water and EtOAc. The layers were separated and the aqueous layer was extracted with EtOAc three times. The combined organic layers were washed with brine, dried on sodium sulfate, filtered and concentrated. The crude material was purified by column chromatography using a gradient of 10-50% EtOAC/Hexane to give 0.50 g of (R)-N-((S,Z)-2-(5-bromo-2-fluoropyridin-3-yl)-4-(2,2-dimethylhydrazono)-1,5,5,5-tetrafluoropentan-2-yl)-2-methylpropane-2-sulfinamide (0.50 g, 1.014 mmol, 68.8% yield). MS m/z=494.9 [M+H]+. Calculated for C16H22BrF5N4OS: 493.3.

後処理

  1. temperaturecooled to −78° C
  2. stirringThe reaction was stirred 3 h at −78° C.
  3. custombefore being quenched with saturated aqueous ammonium chloride at −78° C
  4. temperatureThe mixture was warmed up to room temperature
  5. additiondiluted with water and EtOAc
  6. customThe layers were separated
  7. extractionthe aqueous layer was extracted with EtOAc three times
  8. washThe combined organic layers were washed with brine
  9. customdried on sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customThe crude material was purified by column chromatography

出典と根拠

ORDレコード
ord-f71f2973ff1f4abfacca6be30bdc61fa
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296734B2

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