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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Trifluoroacetic acid → HCID 90220400, 화합물

HRID 2199784
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HRID 2199784 반응식
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][CH2:11][N:10]([C:14]2[S:15][C:16]([NH:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)=[C:17]([C:19](=[O:21])[NH2:20])[N:18]=2)[CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:7][C@@H:8]1[CH2:13][CH2:12][CH2:11][N:10]([C:14]2[S:15][C:16]([NH:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)=[C:17]([C:19]([NH2:20])=[O:21])[N:18]=2)[CH2:9]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 90220485HCID 90220485, 화합물

생성물 1

HCID 90220400HCID 90220400, 화합물수율 102.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of {1-[4-carbamoyl-5-(pyridin-2-ylamino)-thiazol-2-yl]-piperidin-3-yl}-carbamic acid tert-butyl ester (prepared as described in example 1) (359 mg, 0.86 mmol) in dichloromethane (10 mL) was added trifluoroacetic acid (10 mL, 130 mmol) to form a yellow solution. The mixture was stirred at ambient temperature for 30 minutes then evaporated to dryness in vacuo. The residue was taken up in dichloromethane (25 mL) and washed with saturated aqueous sodium hydrogen carbonate (100 mL). The organic layer was separated and the aqueous layer extracted with dichloromethane (5×20 mL) until no further yellow color was extracted in to the organic layer. The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo to give 2-((R)-3-amino-piperidin-1-yl)-5-(pyridin-2-ylamino)-thiazole-4-carboxylic acid amide as a yellow solid (280 mg).

후처리

  1. customto form a yellow solution
  2. customthen evaporated to dryness in vacuo
  3. washwashed with saturated aqueous sodium hydrogen carbonate (100 mL)
  4. customThe organic layer was separated
  5. extractionthe aqueous layer extracted with dichloromethane (5×20 mL) until no further yellow color
  6. extractionwas extracted in to the organic layer
  7. dry with materialThe combined organic extracts were dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8c75653b606543cf856fd8843f261380
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09359345B2

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