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Ammonia → HCID 19981882、化合物

HRID 1460468
ノート
印刷プレビュー

反応式

HRID 1460468 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 19981882HCID 19981882、化合物収率 81%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-affbcde8952f4d48939d42b7064b7f99
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05071841

反応ノート

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