Triethylamine → HCID 14372494、化合物

HRID 1723024ノート

反応式

HRID 1723024 の反応式
Cl.[N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[SH:12])[CH:5]=[CH:4][CH:3]=1.Cl[C:14]1[N:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C(N(CC)CC)C>CO>[N:15]1[CH:16]=[CH:17][CH:18]=[N:19][C:14]=1[S:12][C:10]1[CH:9]=[CH:8][CH:7]=[C:6]2[C:11]=1[N:2]=[CH:3][CH:4]=[CH:5]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 744042-ChloropyrimidineHCID 3082386Quinoline-8-thiol hydrochloride

生成物 1

HCID 14372494HCID 14372494、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 210 mg. (1.06 m mole) of quinoline-8-thiol hydrochloride in 5 ml. of dry methanol was added 128 mg. (1.05 mmol) of 2-chloropyrimidine in 2 ml. of the same solvent followed by 0.148 ml (1 mmol) of dry triethylamine. The reaction mixture was allowed to stir at room temperature overnight followed by the removal of the methanol in vacuo. The residue was partitioned between a saturated sodium bicarbonate solution and ethyl acetate. The organic phase was separated, dried and concentrated. The residue was redissolved in chloroform and concentrated without heat. The residue was triturated with ethyl acetate, filtered and dried, 170 mg., m.p. 165°-168° C.

後処理

  1. customfollowed by the removal of the methanol in vacuo
  2. customThe residue was partitioned between a saturated sodium bicarbonate solution and ethyl acetate
  3. customThe organic phase was separated
  4. customdried
  5. concentrationconcentrated
  6. dissolutionThe residue was redissolved in chloroform
  7. concentrationconcentrated
  8. temperaturewithout heat
  9. customThe residue was triturated with ethyl acetate
  10. filtrationfiltered
  11. customdried

出典と根拠

ORDレコード
ord-39115f5f66bf4fc7873ac3dea8bc284f
出典データセット
uspto-grants-1989_08
特許番号
US04859679

反応ノート

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