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Hydrochloric Acid → HCID 66977453, 화합물

HRID 77098
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HRID 77098 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([CH:16]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([C:28]4[NH:32][C:31]5[CH:33]=[CH:34][CH:35]=[CH:36][C:30]=5[N:29]=4)[CH:22]=3)[CH2:17]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CCOCC>[NH:29]1[C:30]2[CH:36]=[CH:35][CH:34]=[CH:33][C:31]=2[N:32]=[C:28]1[C:23]1[CH:22]=[C:21]([N:18]2[CH2:19][CH2:20][CH:16]([C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[O:15])[CH2:17]2)[CH:26]=[CH:25][C:24]=1[Cl:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66977626HCID 66977626, 화합물

생성물 1

HCID 66977453HCID 66977453, 화합물수율 58.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Method G—Step b To a mixture of 4-{1-[3-(1H-Benzoimidazol-2-yl)-4-chloro-phenyl]-pyrrolidine-3-carbonyl}-piperazine-1-carboxylic acid tert-butyl ester (0.11 g, 0.21 mmol) in dcm (1 mL), 2M HCl in Et2O (4 mL) was added. The mixture was stirred at room temperature overnight, the precipitate obtained was filtered off, and washed with Et2O. The precipitate was then recovered in saturated NaHCO3 solution (3 mL), extracted with dcm (2×3 mL), solvent removed and the crude filtered through an SCX cartridge, to obtain 0.05 g of the title compound (57%).

후처리

  1. additionwas added
  2. customthe precipitate obtained
  3. filtrationwas filtered off
  4. washwashed with Et2O
  5. customThe precipitate was then recovered in saturated NaHCO3 solution (3 mL)
  6. extractionextracted with dcm (2×3 mL), solvent
  7. customremoved
  8. filtrationthe crude filtered through an SCX cartridge

출처 및 근거

ORD 기록
ord-2a0f98412862442fbfc0854041ee8fb7
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08835648B2

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