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1-benzoyl-3-(2-(4,4-dimethyl-3,4-dihydroquinolin-1(2H)-yl)phenyl)thiourea → N-[2-(4,4-Dimethyl-3,4-dihydroquinolin-1(2H)-yl)phenyl]thiourea

HRID 2192214
ノート
印刷プレビュー

反応式

HRID 2192214 の反応式
C([NH:9][C:10]([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:22]([CH3:30])([CH3:29])[CH2:21][CH2:20]1)=[S:11])(=O)C1C=CC=CC=1>CO>[CH3:29][C:22]1([CH3:30])[C:23]2[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:19]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[NH:12][C:10]([NH2:9])=[S:11])[CH2:20][CH2:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 593376891-benzoyl-3-(2-(4,4-dimethyl-3,4-dihydroquinolin-1(2H)-yl)phenyl)thiourea

生成物 1

HCID 59337688N-[2-(4,4-Dimethyl-3,4-dihydroquinolin-1(2H)-yl)phenyl]thiourea

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1e was heated at 80° C. in the presence of MeOH (2.5 mL and 1N NaOH 0.5 mL) for 40 min. LC-MS showed completion of the reaction. The solvent was concentrated, and 1N HCl was added followed by the addition of Et2O. The Et2O layer was separated and was washed with H2O (2×), brine, dried over MgSO4, filtered, and concentrated to dryness. The resulting crude if was used directly in the next step: LC-MS (ESI) 312.1 (M+H) (10-90% MeOH in H2O with 0.1% TFA in a 4 min run, tR=3.51 min).

後処理

  1. custom
completion of the reaction
  • concentrationThe solvent was concentrated
  • addition1N HCl was added
  • additionfollowed by the addition of Et2O
  • customThe Et2O layer was separated
  • washwas washed with H2O (2×), brine
  • dry with materialdried over MgSO4
  • filtrationfiltered
  • concentrationconcentrated to dryness
  • 出典と根拠

    ORDレコード
    ord-cf012dd7d74e41659d6bca23db028843
    出典データセット
    uspto-grants-2012_12
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US08329718B2

    反応ノート

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