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Triethylamine → HCID 86635670, 화합물

HRID 2388709
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HRID 2388709 반응식
[OH:1][CH2:2][C:3]1[S:4][C:5]2[CH2:6][N:7]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:9][C:10]=2[N:11]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>ClCCl>[CH3:26][S:27]([O:1][CH2:2][C:3]1[S:4][C:5]2[CH2:6][N:7]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:9][C:10]=2[N:11]=1)(=[O:29])=[O:28]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 68643978HCID 68643978, 화합물

생성물 1

HCID 86635670HCID 86635670, 화합물수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a dichloromethane solution (15 ml) of tert-butyl 2-(hydroxymethyl)-6,7-dihydrothiazolo[5,4-c]pyridine-5(4H)-carboxylate (1 eq.) was added triethylamine (2.5 eq.) and methane sulfonylchloride (1.2 eq.) at 0° C. and the resulting reaction mixture was stirred at ambient temperature for 2 h. The reaction was quenched with ice and diluted with dichloromethane. The organic layer was successively washed with water and brine and finally dried over sodium sulfate. Evaporation of the organic layer under reduced pressure gave the crude product which was used directly in the next step without further purification. Yield: 80%.

후처리

  1. customthe resulting reaction mixture
  2. customThe reaction was quenched with ice
  3. additiondiluted with dichloromethane
  4. washThe organic layer was successively washed with water and brine
  5. dry with materialfinally dried over sodium sulfate
  6. customEvaporation of the organic layer under reduced pressure

출처 및 근거

ORD 기록
ord-21b3ec9a1c894fe6b4a473f6a62f7456
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268814B2

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