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Hydrochloric Acid → N-benzyl-4-(1-benzylthio-1-methylethyl)-2-ethylidene-4-butanelactam

HRID 2211013
ノート
印刷プレビュー

反応式

HRID 2211013 の反応式
Cl.Br[CH2:3]/[C:4](=[CH:9]\[CH3:10])/[C:5](OC)=[O:6].[CH2:11]([S:18][C:19]([CH3:30])([CH3:29])[CH:20]=[N:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-].[NH4+]>C1COCC1.[Zn]>[CH2:22]([N:21]1[CH:20]([C:19]([S:18][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)([CH3:30])[CH3:29])[CH2:3][C:4](=[CH:9][CH3:10])[C:5]1=[O:6])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=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 25517Ammonium ChlorideHCID 11019705Methyl 2-bromomethylcrotonateHCID 19378136N-(2-benzylthio-2-methylpropylidene)benzylamine

生成物 1

HCID 53674808N-benzyl-4-(1-benzylthio-1-methylethyl)-2-ethylidene-4-butanelactam収率 19%

試薬・触媒・溶媒 2

HCID 23994
Zinc
触媒
HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a stirred suspension of zinc dust (0.53 g) activated with hydrochloric acid in THF (20 ml), methyl 2-bromomethylcrotonate (1.50 g) dissolved in THF (10 ml) and N-(2-benzylthio-2-methylpropylidene)benzylamine (2.00 g) dissolved in THF (10 ml) were added dropwise in the order named at about 30° C. under nitrogen atmosphere and ultrasonic irradiation. The mixture was stirred overnight at room temperature. To the mixture saturated aqueous ammonium chloride solution was added. The mixture was filtered by celite. A reaction product was extracted with ethyl acetate from the filtrate. The organic layer was washed with IN hydrochloric acid, water and then saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The oily residue was purified by silica gel column chromatography to give 1.03 g (40%) of the titled compound No.7-1 and 0.48 g (19%) of the titled compound No.7-2.

後処理

  1. additionwere added dropwise in the order
  2. customnamed at about 30° C. under nitrogen atmosphere
  3. customultrasonic irradiation
  4. filtrationThe mixture was filtered by celite
  5. extractionA reaction product was extracted with ethyl acetate from the filtrate
  6. washThe organic layer was washed with IN hydrochloric acid, water
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customThe oily residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e03ea93b583047caa0a9dd1057e4706b
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05461158

反応ノート

読み込み中…

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