Tetrahydrofuran → HCID 53871027, 화합물

HRID 1419709노트

반응식

HRID 1419709 반응식
C[Mg]Cl.O1CCC[CH2:5]1.Cl[C:10]1[S:11][C:12]2[CH:18]=[C:17]([F:19])[CH:16]=[C:15]([Cl:20])[C:13]=2[N:14]=1.[Cl-].[NH4+]>C(OCC)C.Cl[Ni](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Cl:20][C:15]1[C:13]2[N:14]=[C:10]([CH3:5])[S:11][C:12]=2[CH:18]=[C:17]([F:19])[CH:16]=1

참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 534405702,4-Dichloro-6-fluoro-1,3-benzothiazoleHCID 178418332HCID 178418332, 화합물

생성물 1

HCID 53871027HCID 53871027, 화합물수율 49.6%

시약·촉매·용매 2

HCID 178418751HCID 178418751, 화합물촉매HCID 3283Diethyl Ether용매

실험 절차

67 ml of a solution of methyl magnesium chloride in tetrahydrofuran (3M; 0.2 mol) were added dropwise to a solution of 22 g (0.1 mol) of 2,4-dichloro-6-fluorobenzothiazole and 3.3 g (5 mmol) of dichlorobis(triphenylphosphine)nickel in 100 ml of diethyl ether. After stirring had been carried out for 2 hours, the mixture was poured onto saturated aqueous ammonium chloride solution. The desired product was extracted with diethyl ether, after which the combined organic phases were washed with water, dried over magnesium sulfate and finally evaporated down. 10 g of the desired product were obtained by crystallization from petroleum ether.

후처리

  1. extractionThe desired product was extracted with diethyl ether
  2. washafter which the combined organic phases were washed with water
  3. dry with materialdried over magnesium sulfate
  4. customfinally evaporated down

출처 및 근거

ORD 기록
ord-82e7a942b1ef455fb8614a838e5d0e60
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05888940

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