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Calcium Carbonate → Spiro(benzofuran-2(3H),1'-cyclopropan)-3-one, 5-amino-4-bromo-

HRID 894625
ノート
印刷プレビュー

反応式

HRID 894625 の反応式
[NH2:1][C:2]1[CH:13]=[CH:12][C:5]2[O:6][C:7]3([C:10](=[O:11])[C:4]=2[CH:3]=1)[CH2:9][CH2:8]3.C(=O)([O-])[O-].[Ca+2].[Br:19]Br>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl>[NH2:1][C:2]1[CH:13]=[CH:12][C:5]2[O:6][C:7]3([C:10](=[O:11])[C:4]=2[C:3]=1[Br:19])[CH2:9][CH2:8]3
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10112Calcium CarbonateHCID 24408BromineHCID 12925991HCID 12925991、化合物

生成物 1

HCID 3055477Spiro(benzofuran-2(3H),1'-cyclopropan)-3-one, 5-amino-4-bromo-

試薬・触媒・溶媒 2

HCID 5943Carbon Tetrachloride溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-17 °C

実験手順

5-Aminospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one (0.747 g.) and calcium carbonate (0.47 g.) were suspended in a mixture of carbon tetrachloride (20 ml.) and methylene chloride (5 ml.). The suspension was cooled to -17° C., then bromine (0.22 ml.) was added thereto dropwise, followed by stirring for 45 minutes. The reaction mixture was poured into ice-water, then extracted with ethyl acetate. The extract was washed with water and dried. The solvent was evaporated off, and the residue was recrystallized from ethanol-water. By the above procedure there was obtained 5-amino-4-bromospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one as yellow needles melting at 167°-170° C. Yield 0.6 g.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customThe solvent was evaporated off
  5. customthe residue was recrystallized from ethanol-water

出典と根拠

ORDレコード
ord-e6844d638f9a4e05aa72564fcbfd7946
出典データセット
uspto-grants-1981_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04284644

反応ノート

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