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Hydrazine → HCID 90373274、化合物

HRID 930417
ノート
印刷プレビュー

反応式

HRID 930417 の反応式
[CH3:1][N:2]([CH3:10])/[N:3]=[C:4](\[CH3:9])/[C:5]([F:8])([F:7])[F:6].C([N-]C(C)C)(C)C.[Li+].CCCCCCC.O1CCCC1.C(C1C=CC=CC=1)C.[F:39][CH2:40]/[C:41](=[N:50]/[S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])/[C:42]1[CH:47]=[CH:46][CH:45]=[C:44]([CH3:48])[C:43]=1[F:49].C[Al](C)C.NN>C1COCC1.C1(C)C=CC=CC=1>[CH3:1][N:2]([CH3:10])/[N:3]=[C:4](\[C:5]([F:8])([F:7])[F:6])/[CH2:9][C:41]([NH:50][S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])([C:42]1[CH:47]=[CH:46][CH:45]=[C:44]([CH3:48])[C:43]=1[F:49])[CH2:40][F:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 9321HydrazineHCID 2724682Lithium diisopropylamideHCID 16682925TrimethylaluminumHCID 22742125Tetrahydrofuran heptane ethylbenzolHCID 58668234HCID 58668234、化合物HCID 90373039HCID 90373039、化合物

生成物 1

HCID 90373274
HCID 90373274、化合物
収率 180.9%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (E)-1,1-dimethyl-2-(1,1,1-trifluoropropan-2-ylidene)hydrazine (2.256 g, 14.63 mmol) in dry THF (20 mL) at −78° C. were added n,n,n′,n′-tetramethylethylenediamine (2.190 ml, 14.63 mmol) and lithium diisopropylamide, 2.0m heptane/tetrahydrofuran/ethylbenzene (7.32 ml, 14.63 mmol) and stirred at this temperature for 30 min. A solution of (R,E)-N-(2-fluoro-1-(2-fluoro-3-methylphenyl)ethylidene)-2-methylpropane-2-sulfinamide (2.0 g, 7.32 mmol) in toluene (12 mL) at −78° C. was treated with trimethylaluminum, 2.0m solution in toluene (3.66 ml, 7.32 mmol) for 10 min and added dropwise to the solution containing the hydrazine at −78° C. The resulting mixture was stirred at this temperature for 1.5 h. The mixture was quenched with saturated NH4Cl, and extracted with EtOAc. The combined organics were dried over Na2SO4, filtered, concentrated and chromatographed on silica gel using 0-50% EtOAc/hexanes to afford a bright yellow oil as (R)-N-((Z)-4-(2,2-dimethylhydrazono)-1,5,5,5-tetrafluoro-2-(2-fluoro-3-methylphenyl)pentan-2-yl)-2-methylpropane-2-sulfinamide (5.66 g, 77% yield, combined). MS m/z=427.9 [M+H]+. Calculated for C18H26F5N3OS: 427.17.

後処理

  1. additionadded dropwise to the solution
  2. stirringThe resulting mixture was stirred at this temperature for 1.5 h
  3. customThe mixture was quenched with saturated NH4Cl
  4. extractionextracted with EtOAc
  5. dry with materialThe combined organics were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customchromatographed on silica gel using 0-50% EtOAc/hexanes

出典と根拠

ORDレコード
ord-5a57ae2416624dbb997c43a0eb7e0035
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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