Hydrochloric Acid → HCID 66918867, 화합물

HRID 1279615노트

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HRID 1279615 반응식
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:6]=1[N:15]([S:19]([CH2:22][CH:23](O)[CH2:24][CH2:25][CH2:26][CH3:27])(=[O:21])=[O:20])[CH:16]([CH3:18])[CH3:17].N12CCCCC1CNCC=C2.Cl>C(Cl)Cl.S(Cl)(C)(=O)=O>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:6]=1[N:15]([S:19]([CH:22]=[CH:23][CH2:24][CH2:25][CH2:26][CH3:27])(=[O:20])=[O:21])[CH:16]([CH3:18])[CH3:17]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 22671994HCID 22671994, 화합물HCID 226720701,5-Diazabicyclo[5.4.0]undecene

생성물 1

HCID 66918867HCID 66918867, 화합물수율 91.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 31297Methanesulfonyl chloride용매

실험 절차

To a solution of 2-(N-isopropyl-2-hydroxyhexylsulfonylamino)-5-trifluoromethylphenyl methoxymethyl ether (160 mg; prepared in Reference Example 31.) in methylene chloride (2.0 ml), triethylamine(104 μl) and mesylchloride (35μl) were added in a stream of argon at 0° C. The mixture was stirred for 10 minutes. To the mixture, 1,5-diazabicyclo[5,4,0]undecene (134 μl) was added. The mixture was stirred for 2 hours at room temperature. To the reaction mixture, diluted HCl was added. The mixture was extracted with ethyl acetate, washed, dried over and concentrated with the reduced pressure. The residue was purified on silica gel column chromatography (hexane:AcOEt=8:1) to give the title compound (140 mg) having the following physical data.

후처리

  1. stirringThe mixture was stirred for 2 hours at room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washwashed
  4. customdried over and
  5. concentrationconcentrated with the reduced pressure
  6. customThe residue was purified on silica gel column chromatography (hexane:AcOEt=8:1)

출처 및 근거

ORD 기록
ord-3ad8597c20684e4688a36f96fc6bf195
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06448290B1

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