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

HRID 342448
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HRID 342448 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 782183,6-Dichlorophthalic anhydrideHCID 227253547-Amino-2,3-dimethylbenzo[b]furan

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e3e72c88d0ba412fb5f1891472c05201
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05858995

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