Pyridine → HCID 54491580, 화합물

HRID 648769

반응식

HRID 648769 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 54491580HCID 54491580, 화합물수율 53.5%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e35bdfa6f57408fb75bc914e9662299
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04736055

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