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Ammonia → HCID 19981882, 화합물

HRID 1460468
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HRID 1460468 반응식
[CH3:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]2[CH:10]([C:11](O)=[O:12])[S:9][CH2:8][C:7](=[O:14])[C:6]=2[CH:15]=1.C(Cl)(=O)C(Cl)=O.[NH3:23].C(OCC)(=O)C>C1COCC1.CN(C=O)C>[CH3:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]2[CH:10]([C:11]([NH2:23])=[O:12])[S:9][CH2:8][C:7](=[O:14])[C:6]=2[CH:15]=1
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 8857Ethyl AcetateHCID 65578Oxalyl chlorideHCID 106812951H-2-Benzothiopyran-1-carboxylicacid, 3,4-dihydro-6,7-dimethyl-4-oxo-

생성물 1

HCID 19981882HCID 19981882, 화합물수율 81%

시약·촉매·용매 2

HCID 6228Dimethylformamide
촉매
HCID 8028Tetrahydrofuran용매

실험 절차

In THF (10 ml) was dissolved 6,7-dimethyl3,4-dihydro-1H-2-benzothiopyran-4-one-1-carboxylic acid (0.473 g) followed by addition of oxalyl chloride (0.305 g) and, then, DMF (1 drop). The mixture was stirred at room temperature for 2 hours. This reaction mixture was added to aqueous ammonia (20 ml)--ethyl acetate (40 ml) and the whole mixture was stirred at room temperature for 30 minutes. The ethyl acetate layer was then separated, washed with water, dried (MgSO4) and the solvent was distilled off to give 6,7-dimethyl-3,4-dihydro-1H-2-benzothiopyran-4-one-1-carboxamide (0.38 g, 81%). Recrystallization from ethyl acetate gave colorless plates melting at 197°-198° C.

후처리

  1. customThe ethyl acetate layer was then separated
  2. washwashed with water
  3. dry with materialdried (MgSO4)
  4. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-affbcde8952f4d48939d42b7064b7f99
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05071841

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