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Triethylamine → 7-[(3-Chloro-4-fluoro-2-methylphenyl)carbonyl]-3-(1,2,4-thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine

HRID 1889110
ノート
印刷プレビュー

反応式

HRID 1889110 の反応式
[S:1]1[C:5]([C:6]2[N:10]3[CH2:11][CH2:12][NH:13][CH2:14][C:9]3=[N:8][N:7]=2)=[N:4][CH:3]=[N:2]1.C(N(CC)CC)C.[Cl:22][C:23]1[C:24]([CH3:33])=[C:25]([CH:29]=[CH:30][C:31]=1[F:32])[C:26](Cl)=[O:27].C([O-])(O)=O.[Na+]>C(Cl)Cl.CO.C(OCC)(=O)C>[Cl:22][C:23]1[C:24]([CH3:33])=[C:25]([C:26]([N:13]2[CH2:12][CH2:11][N:10]3[C:6]([C:5]4[S:1][N:2]=[CH:3][N:4]=4)=[N:7][N:8]=[C:9]3[CH2:14]2)=[O:27])[CH:29]=[CH:30][C:31]=1[F:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 665987953-(1,2,4-Thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazineHCID 866667393-Chloro-4-fluoro-2-methylbenzoyl chloride

生成物 1

HCID 665994327-[(3-Chloro-4-fluoro-2-methylphenyl)carbonyl]-3-(1,2,4-thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine

試薬・触媒・溶媒 3

HCID 887Methanol触媒HCID 6344Dichloromethane溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-(1,2,4-thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (I115) (50 mg, 0.240 mmol) and triethylamine (0.050 mL, 0.360 mmol) in DCM (1.5 ml) was treated with 3-chloro-4-fluoro-2-methylbenzoyl chloride (I58) (54.7 mg, 0.264 mmol) in DCM (0.5 ml) and stirred at room temp for 1 h. After 1 h, 2 drops of methanol and then NaHCO3 solution (5 ml) and ethyl acetate (30 ml) were added. The product was extracted into the ethyl acetate which was dried (Na2SO4) and concentrated. Purification by high pH MDAP gave desired product as a white solid in 44 mg.

後処理

  1. waitAfter 1 h
  2. extractionThe product was extracted into the ethyl acetate which
  3. dry with materialwas dried (Na2SO4)
  4. concentrationconcentrated
  5. customPurification by high pH

出典と根拠

ORDレコード
ord-ef6aa19073274985a3639a70e8c82e38
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501946B2

反応ノート

読み込み中…

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