6-morpholin-4-ylpyrazine-2-carboxylic Acid → HCID 178522722、化合物

HRID 414460ノート

反応式

HRID 414460 の反応式
[N:1]1([C:7]2[N:12]=[C:11]([C:13]([OH:15])=O)[CH:10]=[N:9][CH:8]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[NH2:16][C:17]1[NH:21][N:20]=[N:19][N:18]=1>O1CCCC1.C(N(CC)CC)C.C(Cl)(=O)C(C)(C)C>[N:1]1([C:7]2[N:12]=[C:11]([C:13]([NH:16][C:17]3[NH:21][N:20]=[N:19][N:18]=3)=[O:15])[CH:10]=[N:9][CH:8]=2)[CH2:2][CH2:3][O:4][CH2:5][CH2:6]1

参加物

6

反応物 2

HCID 27625626-morpholin-4-ylpyrazine-2-carboxylic AcidHCID 178509299HCID 178509299、化合物

生成物 1

HCID 178522722HCID 178522722、化合物

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 62493Pivaloyl chloride溶媒

実験手順

To a suspension of 2.50 g of 6-(4-morpholinyl) pyrazine-2-carboxylic acid in 50 ml of tetrahydrofuran, 3.60 ml of triethylamine and 1.60 ml of pivaloyl chloride were added dropwise successively at 0° C. under stirring. After stirring for 1 hour at 0° C., 1.12 g of 5-amino-1H-tetrazole was added to the mixture, and the reaction mixture was stirred for 1 hour at room temperature, and then refluxed for 12 hours. The reaction mixture was evaporated, and water was added to the residue. The precipitate was collected by filtration, and recrystalized from a mixture of dimethylsulfoxide and methanol affording 1.74 g of the desired compound as yellow needles. The obtained crystal was consistent with that of (a).

後処理

  1. additionwere added dropwise successively at 0° C.
  2. stirringAfter stirring for 1 hour at 0° C.
  3. stirringthe reaction mixture was stirred for 1 hour at room temperature
  4. temperaturerefluxed for 12 hours
  5. customThe reaction mixture was evaporated
  6. additionwater was added to the residue
  7. filtrationThe precipitate was collected by filtration
  8. customrecrystalized from a mixture of dimethylsulfoxide and methanol affording 1.74 g of the desired compound as yellow needles

出典と根拠

ORDレコード
ord-f9395cf6d381407994d92ae65080620f
出典データセット
uspto-grants-1988_12
特許番号
US04792547

反応ノート

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