Pyridine → HCID 54491580、化合物

HRID 648769

反応式

HRID 648769 の反応式
N1C=CC=CC=1.[OH:7][N:8]=[C:9]([C:12]1[S:13][CH:14]=[CH:15][CH:16]=1)[C:10]#[N:11].[C:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([S:27](Cl)(=[O:29])=[O:28])=[CH:23][CH:22]=1)(=[O:19])[CH3:18].C(OCC)C>CN(C)C1C=CN=CC=1.O1CCCC1>[C:17]([O:20][C:21]1[CH:22]=[CH:23][C:24]([S:27]([O:7][N:8]=[C:9]([C:12]2[S:13][CH:14]=[CH:15][CH:16]=2)[C:10]#[N:11])(=[O:29])=[O:28])=[CH:25][CH:26]=1)(=[O:19])[CH3:18]

参加物

7

反応物 4

HCID 1049PyridineHCID 3283Diethyl EtherHCID 129257104-(Chlorosulfonyl)phenyl acetateHCID 73667355Alpha-Oximino-2-Thienylacetonitrile

生成物 1

HCID 54491580HCID 54491580、化合物収率 53.5%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

200 mg of 4-dimethylaminopyridine and 6.2 g (0.08 mole) of pyridine are added to a solution of 12 g (0.08 mole) of α-hydroxyiminothien-2-ylacetonitrile (3b) in 75 ml of tetrahydrofuran. With cooling to 0° C., a solution of 18.5 g (0.08 mole) of 4-acetoxybenzenesulfonyl chloride (3a) in 30 ml of tetrahydrofuran is added dropwise. The reaction mixture is stirred for 16 hours at room temperature, and 100 ml of diethyl ether are subsequently added. The precipitated salts are removed by filtration and the solution is concentrated by evaporation. The residual crude product is recrystallised from hexane/ethyl acetate, affording 15 g of crystals with a melting point of 114°-115° C.

後処理

  1. customThe precipitated salts are removed by filtration
  2. concentrationthe solution is concentrated by evaporation
  3. customThe residual crude product is recrystallised from hexane/ethyl acetate

出典と根拠

ORDレコード
ord-6e35bdfa6f57408fb75bc914e9662299
出典データセット
uspto-grants-1988_04
特許番号
US04736055

関連ノート

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