Tetrahydrofuran → HCID 53871027、化合物

HRID 1419709ノート

反応式

HRID 1419709 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 53871027HCID 53871027、化合物収率 49.6%

試薬・触媒・溶媒 2

HCID 178418751HCID 178418751、化合物触媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-82e7a942b1ef455fb8614a838e5d0e60
出典データセット
uspto-grants-1999_03
特許番号
US05888940

反応ノート

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