Methyl iodide → HCID 54225997, 화합물

HRID 1277337노트

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HRID 1277337 반응식
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][CH:2]1[CH:7]=[O: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:39])[CH:33]=[CH:34][C:35]([F:38])([F:37])[F:36])[CH3:30].CI.[Cl-].[NH4+]>O1CCCC1>[CH2:29]([O:31][C:32](=[O:39])[CH:33]([CH3:9])[CH:34]([C:2]1([CH:7]=[O:8])[S:3][CH2:4][CH2:5][CH2:6][S:1]1)[C:35]([F:37])([F:38])[F:36])[CH3:30]

참가 물질

9

반응물 7

HCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 25517Ammonium ChlorideHCID 141226Ethyl 4,4,4-trifluorobut-2-enoateHCID 6379761,3-dithiane-2-carboxaldehydeHCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

생성물 1

HCID 54225997HCID 54225997, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
0 °C

실험 절차

A solution of 1.47 g (10 mMole) of 1,3-dithiane-2-carboxaldehyde 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 1.60 g (9.5 mMole) of 3-trifluoromethylacrylic 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 hoursthen 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-35d56d23766d46369a92ab7f9973ecc1
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04277395

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