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Triethylamine → HCID 21467139, 화합물

HRID 1939216
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HRID 1939216 반응식
[Cl:1][C:2]1[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:3]=1[C:4]([N:6]1[CH2:12][CH2:11][CH:10]=[CH:9][C:8]2[S:13][CH:14]=[CH:15][C:7]1=2)=[O:5].C(N(CC)CC)C.[F:28][C:29]1[CH:30]=[CH:31][C:32]([CH3:38])=[C:33]([CH:37]=1)[C:34](Cl)=[O:35]>ClCCl.O>[S:13]1[C:8]2[CH:9]=[CH:10][CH2:11][CH2:12][N:6]([C:4]([C:3]3[CH:16]=[CH:17][C:18]([NH:20][C:34](=[O:35])[C:33]4[CH:37]=[C:29]([F:28])[CH:30]=[CH:31][C:32]=4[CH3:38])=[CH:19][C:2]=3[Cl:1])=[O:5])[C:7]=2[CH:15]=[CH:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 27373835-Fluoro-2-methylbenzoyl chlorideHCID 21467148HCID 21467148, 화합물

생성물 1

HCID 21467139HCID 21467139, 화합물수율 74.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매3회

실험 절차

To a cooled solution of 0.20 g of 4-(2-chloro-4-aminobenzoyl)-5,6-dihydro-4H-thieno [3,2-b]azepine and 137 μl of triethylamine in 3 ml of dichloromethane is added a solution of 0.142 g of 5-fluoro-2-methylbenzoyl chloride in 1 ml of dichloromethane. The mixture is stirred under argon for 2 days and diluted with 30 ml of dichloromethane and 15 ml of H2O. The organic layer is separated and washed with 15 ml each of 2N citric acid, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate, the filter pad washed with dichloromethane and the filtrate evaporated. The residue is crystallized from ethyl acetate to give 0.215 g of white crystals, m.p. 125°-132° C.

후처리

  1. customThe organic layer is separated
  2. washwashed with 15 ml each of 2N citric acid, 1M NaHCO3, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
  5. washthe filter pad washed with dichloromethane
  6. customthe filtrate evaporated
  7. customThe residue is crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-fe9092a15e804860b8e15db484323a19
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05696112

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