Hydrochloric Acid → 1-[5-(1,1-Difluoro-6-aza-spiro[2.5]oct-6-yl)-pyridin-2-yl]-1,2,3,4-tetrahydroquinoxaline

HRID 40548노트

반응식

HRID 40548 반응식
[F:1][C:2]1([F:29])[C:4]2([CH2:9][CH2:8][N:7]([C:10]3[CH:11]=[CH:12][C:13]([N:16]4[C:25]5[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=5)[N:19](C(O)=O)[CH2:18][CH2:17]4)=[N:14][CH:15]=3)[CH2:6][CH2:5]2)[CH2:3]1.Cl>ClCCl.O1CCOCC1>[F:29][C:2]1([F:1])[C:4]2([CH2:9][CH2:8][N:7]([C:10]3[CH:11]=[CH:12][C:13]([N:16]4[C:25]5[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=5)[NH:19][CH2:18][CH2:17]4)=[N:14][CH:15]=3)[CH2:6][CH2:5]2)[CH2:3]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 676057664-[5-(1,1-difluoro-6-aza-spiro[2.5]oct-6-yl)-pyridin-2-yl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid

생성물 1

HCID 676059371-[5-(1,1-Difluoro-6-aza-spiro[2.5]oct-6-yl)-pyridin-2-yl]-1,2,3,4-tetrahydroquinoxaline

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

1.48 g of tert-butyl ester of 4-[5-(1,1-difluoro-6-aza-spiro[2.5]oct-6-yl)-pyridin-2-yl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid is put in 16 mL of dichloromethane. 24 mL of 4M hydrochloric acid in dioxane is added at +4° C. The solution is stirred at room temperature for 4 h and evaporated to dryness. The residue is taken up in a saturated solution of sodium hydrogen carbonate to basic pH. The solution is extracted twice with dichloromethane, washed with water, dried over magnesium sulfate, filtered and evaporated to dryness. 1.4 g of 1-[5-(1,1-difluoro-6-aza-spiro[2.5]oct-6-yl)-pyridin-2-yl]-1,2,3,4-tetrahydroquinoxaline is obtained.

후처리

  1. customevaporated to dryness
  2. extractionThe solution is extracted twice with dichloromethane
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-5d483bc060bf428eac65f282ef3ffcdf
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530473B2

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