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Triethylamine → 7-(3,6-Dichlorophthalimido)-2,3-dimethylbenzo[b]furan

HRID 342448
ノート
印刷プレビュー

反応式

HRID 342448 の反応式
[NH2:1][C:2]1[C:7]2[O:8][C:9]([CH3:12])=[C:10]([CH3:11])[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[Cl:20][C:21]1[CH:31]=[CH:30][C:29]([Cl:32])=[C:23]2[C:24]([O:26][C:27](=O)[C:22]=12)=[O:25]>ClCCl>[Cl:20][C:21]1[CH:31]=[CH:30][C:29]([Cl:32])=[C:23]2[C:24]([N:1]([C:2]3[C:7]4[O:8][C:9]([CH3:12])=[C:10]([CH3:11])[C:6]=4[CH:5]=[CH:4][CH:3]=3)[C:27](=[O:26])[C:22]=12)=[O:25]
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 8471TriethylamineHCID 782183,6-Dichlorophthalic anhydrideHCID 227253547-Amino-2,3-dimethylbenzo[b]furan

生成物 1

HCID 599198757-(3,6-Dichlorophthalimido)-2,3-dimethylbenzo[b]furan収率 69.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 7-amino-2,3-dimethylbenzo[b]furan (161 mg), triethylamine (202 mg) and 3,6-dichlorophthalic anhydride (261 mg) in dichloromethane (5 ml) was stirred at ambient temperature for 1 hour. The reaction mixture was washed with 1N-hydrochloric acid and brine, dried over sodium sulfate and concentrated in vacuo. The residue was dissolved in methanol and treated with diazomethane. The separated solid was collected and washed with methanol to give 7-(3,6-dichlorophthalimido)-2,3-dimethylbenzo[b]furan (250 mg).

後処理

  1. washThe reaction mixture was washed with 1N-hydrochloric acid and brine
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in methanol
  5. additiontreated with diazomethane
  6. customThe separated solid was collected
  7. washwashed with methanol

出典と根拠

ORDレコード
ord-e3e72c88d0ba412fb5f1891472c05201
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05858995

反応ノート

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