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Dimethyl Sulfoxide → (S,4E)-3-(tert-Butyldimethylsilyloxy)-4-methyl-5-(2-methyl-thiazol-4-yl)-pent-4-enal

HRID 1700960
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HRID 1700960 반응식
CS(C)=O.C(Cl)(=O)C(Cl)=O.[Si:11]([O:18][C@H:19](/[C:23](/[CH3:31])=[CH:24]/[C:25]1[N:26]=[C:27]([CH3:30])[S:28][CH:29]=1)[CH2:20][CH2:21][OH:22])([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12].C(N(CC)CC)C>ClCCl.O>[Si:11]([O:18][C@H:19](/[C:23](/[CH3:31])=[CH:24]/[C:25]1[N:26]=[C:27]([CH3:30])[S:28][CH:29]=1)[CH2:20][CH:21]=[O:22])([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:12])[CH3:13]
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참가 물질

7

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HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 10936330(-)-(3S,4E)-3-{[tert-Butyl(dimethyl)silyl]oxy}-4-methyl-5-(2-methyl-1,3-thiazol-4-yl)pent-4-en-1-ol

생성물 1

HCID 11045612(S,4E)-3-(tert-Butyldimethylsilyloxy)-4-methyl-5-(2-methyl-thiazol-4-yl)-pent-4-enal수율 82.2%

시약·촉매·용매 2

HCID 962Water용매
HCID 6344Dichloromethane용매3회

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온도
-78 °C

실험 절차

A solution of dimethyl sulfoxide (2,04 ml, 28.8 mmol, 2.4 equiv) in 6.0 ml of dichloromethane is added dropwise within 5 min to a stirred solution of oxalyl chloride (1.14 ml, 13.2 mmol, 1.1 equiv) in 30 ml of dichloromethane cooled to −78° C. The mixture is stirred for 10 min at −70° C. A solution of (S,4E)-3-(tert-butyldimethylsilyloxy)-1-hydroxy-4-methyl-5-(2-methylthiazol-4-yl)-pent-4-ene 16 (3.93 g, 12.0 mmol) in 5 ml of dichloromethane is added dropwise within 5 min. The mixture is stirred for 30 min at −70° C. The reaction is quenched by dropwise addition of triethyl amine (8.4 ml, 60.0 mmol). The mixture is warmed to r.t. within 45 min. Water (30 ml) is added and the mixture is stirred for 10 min. The organic layer is seperated and the aqueous layer is extracted with dichloromethane (3×100 ml). The combined organic extracts are dried over magnesium sulfate and concentrated in vacuo. Purification of the residue by flash column chromatography (pentane/diethyl ether 5:2) affords (S,4E)-3-(tert-butyadimethylsilyloxy)-4-methyl-5-(2-methylthiazol-4-yl)-pent-4en-1-al 17 (3.21 g, 82%) as a pale yellow oil.

후처리

  1. stirringThe mixture is stirred for 30 min at −70° C
  2. temperatureThe mixture is warmed to r.t. within 45 min
  3. stirringthe mixture is stirred for 10 min
  4. customThe organic layer is seperated
  5. extractionthe aqueous layer is extracted with dichloromethane (3×100 ml)
  6. dry with materialThe combined organic extracts are dried over magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customPurification of the residue by flash column chromatography (pentane/diethyl ether 5:2)

출처 및 근거

ORD 기록
ord-0b1aecd625f3441f91906c3800560430
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350878B1

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