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Triethylamine → 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

HRID 2308936
ノート
印刷プレビュー

反応式

HRID 2308936 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][CH2:8][C:7](=[O:11])[C:6]=2[CH:12]=1.CO[CH:15](OC)[N:16]([CH3:18])[CH3:17].C(N(CC)CC)C>C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8](=[CH:15][N:16]([CH3:18])[CH3:17])[C:7](=[O:11])[C:6]=2[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 2480656-Chlorothiochroman-4-one

生成物 1

HCID 38135366-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 6-chloro-2,3-dihydro-4H-1-benzothiopyran-4-one (30 g), N,N-dimethylformamide dimethyl acetal (80 ml), and triethylamine (31.4 ml) in benzene (400 ml) was refluxed with stirring for 1 hour and then about three-fourths of the solvent were distilled slowly at atmospheric pressure over a period of approximately 1 hour. Benzene (300 ml) was added to the reaction mixture and the solvent was distilled again. To the residue was added diethyl ether (150 ml) and the mixture was triturated to give 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one (34 g).

後処理

  1. distillationabout three-fourths of the solvent were distilled slowly at atmospheric pressure over a period of approximately 1 hour
  2. additionBenzene (300 ml) was added to the reaction mixture
  3. distillationthe solvent was distilled again
  4. additionTo the residue was added diethyl ether (150 ml)
  5. customthe mixture was triturated

出典と根拠

ORDレコード
ord-e9d86e1fce0949b381afb289ab19606f
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04692444

反応ノート

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