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Methyl iodide → HCID 53760192, 화합물

HRID 1277342
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HRID 1277342 반응식
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][CH:2]1[C:7]#[N:8].[CH:9]([N-]C(C)C)(C)C.[Li+].C(NC(C)C)(C)C.C([Li])CCC.[CH2:29]([O:31][C:32](=[O:37])[CH:33]=[CH:34][CH2:35][F:36])[CH3:30].CI.[Cl-].[NH4+]>O1CCCC1>[CH2:29]([O:31][C:32](=[O:37])[CH:33]([CH3:9])[CH:34]([C:2]1([C:7]#[N:8])[S:3][CH2:4][CH2:5][CH2:6][S:1]1)[CH2:35][F:36])[CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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9

반응물 7

HCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 9728Ethyl 4-fluorobut-2-enoateHCID 25517Ammonium ChlorideHCID 3118391,3-Dithiane-2-carbonitrileHCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

생성물 1

HCID 53760192HCID 53760192, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
0 °C

실험 절차

A solution of 1.45 g (10 mMole) of 1,3-dithian-2-carbonitrile in 10 ml of tetrahydrofuran is added to lithium diisopropylamide, prepared from diisopropylamine (1.01 g, 10 mMole) and butyllithium (4.8 ml of a 2.1 M solution, 10 mM) in 20 ml of tetrahydrofuran at -70° C. To the solution is added 1.25 g (9,5 mMole) of 3-monofluoromethylacrylic acid ethyl ester in 5 ml of tetrahydrofuran and the reaction mixture is stirredat -70° C. for 30 minutes after which 1.3 g (10 mMole) of methyl iodide is added and the mixture is maintained at 0° C. for 15 hours, then poured into aqueous ammonium chloride and extracted with ether. The ether solution is dried and evaporated to give the title compound.

후처리

  1. extractionextracted with ether
  2. dry with materialThe ether solution is dried
  3. customevaporated

출처 및 근거

ORD 기록
ord-4111cf2876f04d50b243b775774c20af
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04277395

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