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Toluene → HCID 21442848、化合物

HRID 1606511
ノート
印刷プレビュー

反応式

HRID 1606511 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][OH:16])[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[C:17]12[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=1)[NH:22]C(=O)O[C:18]2=[O:19].C1(C)C=CC=CC=1>CCOCC>[C:18]([O:16][CH2:15][CH2:14][N:11]1[CH2:10][CH2:9][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)[CH2:13][CH2:12]1)(=[O:19])[C:17]1[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=1)[NH2:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1140TolueneHCID 8359Isatoic AnhydrideHCID 967031-Piperazineethanol, 4-(3-chlorophenyl)-

生成物 1

HCID 21442848HCID 21442848、化合物収率 70%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

7.2 G. (0.03 mol) of 2-(4-m-chlorophenyl-piperazino)-ethanol and 6.55 g. (0.04 mol) of isatoic anhydride in 125 ml. of toluene are refluxed for 3 hours. The hot toluene solution is filtered and the toluene is evaporated from the filtrate to give a residue which is taken up in ether in order to remove a small amount of unreacted isatoic anhydride, the solution is filtered and the ether is driven off. The remaining product is triturated in petroleum ether, filtered off and recrystallised twice from isopropyl alcohol to give 7.6 g. (yield = 70%) of 2-(4-m-chlorophenylpiperazino)-ethyl anthranilate, which melts at 76°C.

後処理

  1. filtrationThe hot toluene solution is filtered
  2. customthe toluene is evaporated from the filtrate
  3. customto give a residue which
  4. customto remove a small amount of unreacted isatoic anhydride
  5. filtrationthe solution is filtered
  6. customThe remaining product is triturated in petroleum ether
  7. filtrationfiltered off
  8. customrecrystallised twice from isopropyl alcohol
  9. customto give 7.6 g

出典と根拠

ORDレコード
ord-3b06104217764322b5bb29aebb5a013c
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03953449

反応ノート

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