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Triethylamine → HCID 21476237, 화합물

HRID 2293288
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HRID 2293288 반응식
[CH:1]1[C:10]2[C:9]3[CH2:11][CH2:12][CH:13]=[CH:14][C:8]=3[N:7]=[CH:6][CH2:5][C:4]=2[S:3][CH:2]=1.[CH3:15][C:16]1[CH:33]=[CH:32][CH:31]=[CH:30][C:17]=1[C:18]([NH:20][C:21]1[CH:29]=[CH:28][C:24]([C:25](Cl)=[O:26])=[CH:23][CH:22]=1)=[O:19].C(N(CC)CC)C>C(Cl)Cl>[CH:1]1[C:10]2[C:9]3[CH2:11][CH:12]([C:25]([C:24]4[CH:23]=[CH:22][C:21]([NH:20][C:18](=[O:19])[C:17]5[CH:30]=[CH:31][CH:32]=[CH:33][C:16]=5[CH3:15])=[CH:29][CH:28]=4)=[O:26])[CH:13]=[CH:14][C:8]=3[N:7]=[CH:6][CH2:5][C:4]=2[S:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 107074414-[(2-methylbenzoyl)amino]benzoyl ChlorideHCID 18929554HCID 18929554, 화합물

생성물 1

HCID 21476237HCID 21476237, 화합물수율 59.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 400 mg of 9,10-dihydro-4H-thieno[2,3-d][1]benzazepine and 600 mg of 4-[(2-methylbenzoyl)amino]benzoyl chloride is stirred in 30 ml of methylene chloride in the presence of 3 ml of triethylamine for 8 hours. The volatiles are removed in vacuo to give a residue which is partitioned between water and chloroform. The organic layer is dried (Na2 SO4) and the filtrate evaporated in vacuo to give a residue which is purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane to give 518 mg of the desired product. M+1=439.

후처리

  1. customThe volatiles are removed in vacuo
  2. customto give a residue which
  3. customis partitioned between water and chloroform
  4. customThe organic layer is dried (Na2 SO4)
  5. customthe filtrate evaporated in vacuo
  6. customto give a residue which
  7. customis purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-64c3e8045bf441c397c3dc4a8de856ff
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05686445

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