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

HRID 21728

반응식

HRID 21728 반응식
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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-4a8947eb6a0041508dc83e1f4689d2d3
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424443

연결된 노트

불러오는 중…