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Dichloromethane → HCID 18796731、化合物

HRID 1938522
ノート
印刷プレビュー

反応式

HRID 1938522 の反応式
C([O:3][C:4]([C:6]1[N:15]=[C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]3[O:24][CH2:25][O:26][C:20]=3[CH:19]=2)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:27])[CH:12]=2)[N:7]=1)=O)C.C(Cl)Cl.O1CCCC1.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1.CO>[CH:4]([C:6]1[N:15]=[C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]3[O:24][CH2:25][O:26][C:20]=3[CH:19]=2)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:27])[CH:12]=2)[N:7]=1)=[O:3]
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 6344DichloromethaneHCID 8028TetrahydrofuranHCID 18796730HCID 18796730、化合物HCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 18796731HCID 18796731、化合物収率 63%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 1140
Toluene
溶媒

実験手順

0.50 g (0.0013 mol) of 2-ethoxycarbonyl-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline was dissolved in a solvent mixture comprising 20 ml of methylene chloride and 20 ml of tetrahydrofuran. 2.6 ml of a 1.0M solution of diisobutylaluminum hydride in toluene was dropped into the solution prepared above at -78° C. under stirring. The obtained mixture was stirred at -78° C. for several hours, followed by the addition of 20 ml of methanol. The obtained mixture was distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography and recrystallized from ethyl acetate/n-hexane to give 0.28 g of the title compound as a pale-yellow crystal.

後処理

  1. customprepared above at -78° C.
  2. stirringThe obtained mixture was stirred at -78° C. for several hours
  3. distillationThe obtained mixture was distilled under a reduced pressure
  4. customto remove the solvent
  5. customThe residue was purified by silica gel column chromatography
  6. customrecrystallized from ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-e47015f4be2c414b8e5d4408dd20569a
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05693652

反応ノート

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