2-Amino-4,5,6,7-tetrahydrobenzothiazole → 2-methylsulfanyl-4-oxo-5,6,7,8-tetrahydro-4H-9-thia-1,4a-diaza-fluorene-3-carboxylic acid

HRID 44444

反応式

HRID 44444 の反応式
[S:1]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:4]=2[N:3]=[C:2]1[NH2:10].[CH2:11]([S:13][C:14](SCC)=[C:15]1[C:20](=O)[O:19]C(C)(C)[O:17][C:16]1=[O:24])C>C(O)C>[CH3:11][S:13][C:14]1[N:10]=[C:2]2[N:3]([C:20](=[O:19])[C:15]=1[C:16]([OH:24])=[O:17])[C:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=1[S:1]2

参加物

4

反応物 2

HCID 180462-Amino-4,5,6,7-tetrahydrobenzothiazoleHCID 136798125-[Bis(ethylsulfanyl)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 671171072-methylsulfanyl-4-oxo-5,6,7,8-tetrahydro-4H-9-thia-1,4a-diaza-fluorene-3-carboxylic acid収率 46.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
87.5 °C

実験手順

The suspension of 4,5,6,7-tetrahydro-benzothiazol-2-yl-amine (8 gm, 0.0519 mol) and 5-(bis-ethylsulfanyl-methylene)-2,2-dimethyl-[1,3]dioxane-4,6-dione (14.2 gm, 0.0572 mol) in ethanol (60 ml) was heated at 85-90° C. for 10 hours. Reaction mixture was cooled to room temperature and filtered. The solid, thus obtained, was washed with ethanol (20 ml) followed by with diethyl ether (50 ml) and suck dried to give 7.2 gm of title compound as a solid.

後処理

  1. customReaction mixture
  2. temperaturewas cooled to room temperature
  3. filtrationfiltered
  4. customThe solid, thus obtained
  5. washwas washed with ethanol (20 ml)
  6. customsuck dried

出典と根拠

ORDレコード
ord-56678c351f3a4011bd521278eac3355d
出典データセット
uspto-grants-2013_09
特許番号
US08541430B2

関連ノート

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