Sodium hydride → HCID 21109460, 화합물

HRID 1766124

반응식

HRID 1766124 반응식
[H-].[Na+].[Cl-].[CH3:4][O:5][C:6]1[CH:31]=[CH:30][C:9]([CH2:10][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:8][C:7]=1[CH3:32].[O:33]1[CH2:38][CH2:37][CH2:36][CH2:35][CH:34]1[O:39][CH2:40][C:41]1[N:42]=[C:43]([C:48]2[CH:53]=[CH:52][C:51]([C:54]([F:57])([F:56])[F:55])=[CH:50][CH:49]=2)[S:44][C:45]=1[CH:46]=O>C(Cl)Cl.C(Cl)(Cl)(Cl)Cl>[CH3:4][O:5][C:6]1[CH:31]=[CH:30][C:9](/[CH:10]=[CH:46]/[C:45]2[S:44][C:43]([C:48]3[CH:53]=[CH:52][C:51]([C:54]([F:56])([F:57])[F:55])=[CH:50][CH:49]=3)=[N:42][C:41]=2[CH2:40][O:39][CH:34]2[CH2:35][CH2:36][CH2:37][CH2:38][O:33]2)=[CH:8][C:7]=1[CH3:32]

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 211094534-[(tetrahydro-2H-pyran-2-yloxy)methyl]-2-[4-(trifluoromethyl)phenyl]-1,3-thiazole-5-carbaldehydeHCID 461800353-Methyl-4-methoxybenzyl triphenylphosphonium chloride

생성물 1

HCID 21109460HCID 21109460, 화합물수율 100%

시약·촉매·용매 2

HCID 5943Carbon Tetrachloride용매HCID 6344Dichloromethane용매

실험 절차

To a suspension of NaH (60% dispersion in mineral oil, 242 mg, 6.32 mmoles, 1.4 eq) in dry CH2Cl2 (15 ml) was added (4-Methoxy-3-methylbenzyl)(triphenyl)phosphonium chloride (2.62 g, 6.32 mmoles, 1.4 eq). This was allowed to stir at room temperature for 1.5 hours followed by the dropwise addition of 4-[(tetrahydro-2H-pyran-2-yloxy)methyl]-2-[4-(trifluoromethyl)phenyl]-1,3-thiazole-5-carbaldehyde (1.68 g, 4.51 mmoles, 1 eq) in anhydrous carbon tetrachloride (25 ml). The resulting reaction mixture was refluxed overnight at which point (after cooling to room temperature) the reaction was washed with 1N NaOH, H2O, brine, dried over Na2SO4 and concentrated in vacuo to yield a >100% yield of a light green oil. The crude material was used without purification.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed overnight at which point (after cooling to room temperature) the reaction
  3. washwas washed with 1N NaOH, H2O, brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-10452da0fe5a4d5c9bdcb7c2c92bd93d
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229998B2

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