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Tetrahydrofuran → HCID 53859638, 화합물

HRID 1086378
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HRID 1086378 반응식
[CH2:1]([C:7]1[CH:8]=[C:9]([C:13]2OCC(C)(C)N=2)[CH:10]=[CH:11][CH:12]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C([Li])(CC)C.C(=O)=[O:26].[C:28](#[N:30])C.CS[S:33][CH3:34].[NH4+].[Cl-].C1C[O:40][CH2:39][CH2:38]1>>[CH3:34][S:33][C:10]1[CH:11]=[CH:12][C:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])=[CH:8][C:9]=1[CH:13]=[CH:38][C:39]([N:30]([OH:26])[CH3:28])=[O:40]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 6

HCID 8028Tetrahydrofuran2회HCID 12232Dimethyl DisulfideHCID 25517Ammonium ChlorideHCID 19827203HCID 19827203, 화합물HCID 86587134Acetonitrile dry iceHCID 178418400CID 53628100

생성물 1

HCID 53859638HCID 53859638, 화합물

실험 절차

To a solution of 2-(3-n-hexylphenyl)-4,4-dimethyl-oxazoline (21 g, 0.086 mmol) in 200 ml of dry THF is added dropwise, sec-butyllithium (73 ml) at a temperature of -40° C. (dry ice/acetonitrile bath). After stirring one hour at -40° C. a solution of dimethyldisulfide (8.18 g, 0.087 mmol) in THF (7.82 ml) is then added dropwise to the reaction mixture and stirred for 2 hours while keeping the temperature at -40° C. The reaction mixture is poured into saturated NH4Cl and then extracted with ethyl acetate. The extracts are washed with water and then brine, dried over MgSO4 and concentrated to afford the subtitle compound.

후처리

  1. additionis then added dropwise to the reaction mixture
  2. customat -40° C
  3. extractionextracted with ethyl acetate
  4. washThe extracts are washed with water
  5. dry with materialbrine, dried over MgSO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2b34307217df4f96b238124e9db30119
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05028629

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