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1,1'-Carbonyldiimidazole → HCID 57991920、化合物

HRID 2075333
ノート
印刷プレビュー

反応式

HRID 2075333 の反応式
[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]2[S:8][C:9]([C:11]([OH:13])=O)=[CH:10][C:3]=12.C1N=CN(C(N2C=NC=C2)=O)C=1.[NH2:26][NH:27][C:28]([NH2:30])=[S:29]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]2[S:8][C:9]([C:11]([NH:26][NH:27][C:28]([NH2:30])=[S:29])=[O:13])=[CH:10][C:3]=12
参加物反応条件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 682631,1'-CarbonyldiimidazoleHCID 2723789ThiosemicarbazideHCID 185161084-Chlorothieno[2,3-c]pyridine-2-carboxylic acid

生成物 1

HCID 57991920HCID 57991920、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
70 °C

実験手順

4-Chlorothieno[2,3-c]pyridine-2-carboxylic acid (4.2 g, 19.7 mmol) was dissolved in 110 mL DMF in a round bottom flask. To this flask was added CDI (7.68 g, 47.4 mmol). After the flask was heated at 70° C. for 30 minutes, thiosemicarbazide (4.32 g, 47.4 mmol) dissolved in 5 mL DMF was added and the resulting mixture was heated at 70° C. for 30 minutes. After removing the DMF under reduced pressure, the remaining residue was mixed with 50 mL 1N HCl. After filtration and washing with water, the product was dried in a vacuum oven at 80° C. for 4 hours. The resulting product (6.0 g) was used directly in the next step. LCMS (API-ES) m/z (%): 287.1 (100%, M++H).

後処理

  1. additionwas added
  2. temperaturethe resulting mixture was heated at 70° C. for 30 minutes
  3. customAfter removing the DMF under reduced pressure
  4. additionthe remaining residue was mixed with 50 mL 1N HCl
  5. filtrationAfter filtration
  6. washwashing with water
  7. customthe product was dried in a vacuum oven at 80° C. for 4 hours

出典と根拠

ORDレコード
ord-037c22bdd4e64189ad0595131106d543
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919504B2

反応ノート

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