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Hydrochloric Acid → (RS)-S-(4-aminophenyl)-S-cyclopropyl-N-[2-(trimethylsilyl)ethylsulfonyl]sulfoximide

HRID 1891076
ノート
印刷プレビュー

反応式

HRID 1891076 の反応式
[CH:1]1([S:4]([C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][CH:17]=2)(=[N:6][S:7]([CH2:10][CH2:11][Si:12]([CH3:15])([CH3:14])[CH3:13])(=[O:9])=[O:8])=[O:5])[CH2:3][CH2:2]1.Cl.[OH-].[Na+].C(OCC)(=O)C>O1CCCC1.[Cl-].[Ti+3].[Cl-].[Cl-]>[NH2:22][C:19]1[CH:20]=[CH:21][C:16]([S:4]([CH:1]2[CH2:3][CH2:2]2)(=[N:6][S:7]([CH2:10][CH2:11][Si:12]([CH3:14])([CH3:15])[CH3:13])(=[O:8])=[O:9])=[O:5])=[CH:17][CH:18]=1
参加物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 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 59252685(RS)-S-cyclopropyl-S-(4-nitrophenyl)-N-[2-(trimethylsilyl)ethyl-sulfonyl]sulfoximide

生成物 1

HCID 59674073(RS)-S-(4-aminophenyl)-S-cyclopropyl-N-[2-(trimethylsilyl)ethylsulfonyl]sulfoximide収率 72.8%

試薬・触媒・溶媒 2

HCID 10313229
titanium(III) trichloride
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

320 mg of (RS)—S-cyclopropyl-S-(4-nitrophenyl)-N-[2-(trimethylsilyl)ethyl-sulfonyl]sulfoximide is dissolved in 5 ml of tetrahydrofuran. While being cooled with ice, 7.2 ml of an approximately 10% by weight solution of titanium(III) chloride in 20-30% by weight of hydrochloric acid is added in drops. The solution is stirred for 16 hours at room temperature and poured onto ice. The pH is set at 8-9 with 15% sodium hydroxide solution. After ethyl acetate is added, the mixture is vigorously stirred. The precipitate is suctioned off and washed with 100 ml of ethyl acetate. The filtrates are combined, dried and concentrated by evaporation. After purification by flash chromatography, 215 mg of (RS)—S-(4-aminophenyl)-S-cyclopropyl-N-[2-(trimethylsilyl)ethylsulfonyl]sulfoximide is obtained.

後処理

  1. additionis added in drops
  2. additionpoured onto ice
  3. stirringthe mixture is vigorously stirred
  4. washwashed with 100 ml of ethyl acetate
  5. customdried
  6. concentrationconcentrated by evaporation
  7. customAfter purification by flash chromatography

出典と根拠

ORDレコード
ord-a55717aa56604bed9e9ef8efe970613c
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507510B2

反応ノート

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