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Triethylamine → HCID 9821613、化合物

HRID 2212344
ノート
印刷プレビュー

反応式

HRID 2212344 の反応式
C(N(CC)CC)C.Br.Br[CH:10]([C:21]1[CH:26]=[CH:25][N:24]=[C:23]([O:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:22]=1)[C:11]([C:13]1[CH:18]=[C:17]([CH3:19])[CH:16]=[C:15]([CH3:20])[CH:14]=1)=O.[NH2:35][C:36]([NH2:38])=[S:37]>C(#N)C>[CH3:20][C:15]1[CH:14]=[C:13]([C:11]2[N:35]=[C:36]([NH2:38])[S:37][C:10]=2[C:21]2[CH:26]=[CH:25][N:24]=[C:23]([O:27][CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[CH:22]=2)[CH:18]=[C:17]([CH3:19])[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 21964198HCID 21964198、化合物

生成物 1

HCID 9821613HCID 9821613、化合物収率 53.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Triethylamine (1.4 mL, 10 mmol) was added dropwise to a solution of 2-bromo-1-(3,5-dimethylphenyl)-2-(2-phenylmethyloxy-4-pyridyl)ethanone hydrobromide (4.8 g, 9.8 mmol) and thiourea (0.77 g, 11 mmol) in acetonitrile (40 mL) and the mixture was stirred at room temperature for 3 hours. The solvent was removed under reduced pressure, a saturated aqueous solution of sodium hydrogencarbonate was added to the residue and extracted with ethyl acetate. The organic layer was washed with water, dried and the solvent was distilled off. The resulting crude crystals were recrystallized from ethyl acetate to obtain 2.0 g (5.2 mmol, yield 53%) of the title compound.

後処理

  1. customThe solvent was removed under reduced pressure
  2. additiona saturated aqueous solution of sodium hydrogencarbonate was added to the residue
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. customdried
  6. distillationthe solvent was distilled off
  7. customThe resulting crude crystals were recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-c3ab1b3dabe44fa6b83ac293c3b95bbf
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07101899B1

反応ノート

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