Thiophosgene → 2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole

HRID 21728

反応式

HRID 21728 の反応式
C(=O)([O-])[O-].[Ca+2].[C:6](Cl)(Cl)=[S:7].[NH2:10][C:11]1[C:19]2[S:18][C:17]([Cl:20])=[N:16][C:15]=2[C:14]([Cl:21])=[CH:13][C:12]=1[F:22]>O.ClCCl>[Cl:20][C:17]1[S:18][C:19]2[C:11]([N:10]=[C:6]=[S:7])=[C:12]([F:22])[CH:13]=[C:14]([Cl:21])[C:15]=2[N:16]=1

参加物

6

反応物 3

HCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 199334577-Amino-2,4-dichloro-6-fluorobenzothiazole

生成物 1

HCID 199334642,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

A suspension of 16.9 g calcium carbonate in 100 ml water was added to a solution of 19.4 g thiophosgene in 100 ml dichloromethane. A solution of 40 g 7-amino-2,4-dichloro-6-fluorobenzothiazole in 500 ml dichloromethane was added, dropwise at 5° C., and the mixture stirred for 8 hours at room temperature. The solid was filtered, the phases were separated, and the organic phase dried over magnesium sulfate and concentrated. The residue was purified by column chromatography (eluent: hexane/ethyl acetate). Yield: 16 g=38% of theory m.p.: 80°-81° C.

後処理

  1. filtrationThe solid was filtered
  2. customthe phases were separated
  3. dry with materialthe organic phase dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (eluent: hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4a8947eb6a0041508dc83e1f4689d2d3
出典データセット
uspto-grants-1995_06
特許番号
US05424443

関連ノート

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