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

HRID 40548ノート

反応式

HRID 40548 の反応式
[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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5d483bc060bf428eac65f282ef3ffcdf
出典データセット
uspto-grants-2013_09
特許番号
US08530473B2

反応ノート

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