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Hydrochloric Acid → HCID 68830378, 화합물

HRID 747758
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HRID 747758 반응식
Cl.[CH2:2]([O:9][C:10]([N:12]1[CH2:17][CH2:16][CH:15]([O:18][C:19]2[CH:24]=[CH:23][C:22]([CH2:25][C@H:26]([NH:37]C(OC(C)(C)C)=O)[CH2:27][O:28][C:29]3[CH:30]=[C:31]([CH:34]=[CH:35][CH:36]=3)[C:32]#[N:33])=[CH:21][CH:20]=2)[CH2:14][CH2:13]1)=[O:11])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(C(C)C)CC)(C)C.[I:54][C:55]1[CH:60]=[CH:59][C:58]([S:61](Cl)(=[O:63])=[O:62])=[CH:57][CH:56]=1>O1CCOCC1.C(OCC)(=O)C>[CH2:2]([O:9][C:10]([N:12]1[CH2:13][CH2:14][CH:15]([O:18][C:19]2[CH:24]=[CH:23][C:22]([CH2:25][C@H:26]([NH:37][S:61]([C:58]3[CH:59]=[CH:60][C:55]([I:54])=[CH:56][CH:57]=3)(=[O:63])=[O:62])[CH2:27][O:28][C:29]3[CH:30]=[C:31]([CH:34]=[CH:35][CH:36]=3)[C:32]#[N:33])=[CH:21][CH:20]=2)[CH2:16][CH2:17]1)=[O:11])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 73994-Iodobenzenesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 68829666HCID 68829666, 화합물

생성물 1

HCID 68830378HCID 68830378, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매
HCID 31275
1,4-Dioxane
용매
2회

실험 절차

25 ml of 4 N solution of hydrogen chloride in dioxane and 12.5 ml of dioxane were added to 2.54 g (4.34 mmol) of 3-[(2S)-3-[4-[1-(benzyloxycarbonyl)-4-piperidyloxy]phenyl]-2-(t-butoxycarbonylamino)propoxy]benzonitrile. After stirring at room temperature for 24 hours, the solvent was distilled off under reduced pressure. The residue was dissolved in 40 ml of DMF. 1.77 ml (13.0 mmol) of diisopropylethylamine and 1.97 g (6.51 mmol)) of 4-iodobenzenesulfonyl chloride were added to the solution at 0° C. 30 minutes after, the temperature was elevated to room temperature, and the reaction mixture was stirred for 19 hours. Ater the same isolation process as that of step 1 in Example 1 with ethyl acetate as the extractant, the crude product was obtained, which was purified by the silica gel column chromatography to obtain the title compound.

후처리

  1. distillationthe solvent was distilled off under reduced pressure
  2. dissolutionThe residue was dissolved in 40 ml of DMF
  3. custom30 minutes
  4. customwas elevated to room temperature
  5. stirringthe reaction mixture was stirred for 19 hours
  6. customwhich was purified by the silica gel column chromatography

출처 및 근거

ORD 기록
ord-7064968bbb004e1d82d9ecce9e099775
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07396844B1

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