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Pyridine → HCID 59623756、化合物

HRID 1093948
ノート
印刷プレビュー

反応式

HRID 1093948 の反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:22])(=[O:21])[NH:12][C:13]2[C:18]([C:19]=1[OH:20])=[N:17][CH:16]=[CH:15][N:14]=2.N1C=CC=CC=1.[CH3:29][C:30]([CH3:35])([CH3:34])[C:31](Cl)=[O:32]>ClCCl>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:21])(=[O:22])[NH:12][C:13]2[C:18]([C:19]=1[O:20][C:31](=[O:32])[C:30]([CH3:35])([CH3:34])[CH3:29])=[N:17][CH:16]=[CH:15][N:14]=2
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 1049PyridineHCID 62493Pivaloyl chlorideHCID 59623744HCID 59623744、化合物

生成物 1

HCID 59623756HCID 59623756、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
40 °C

実験手順

To a suspension of Compound No. A2 (Example 3.1) in dichloromethane (10 ml) was added pyridine (0.205 ml) followed by 2,2-dimethylpropionyl chloride (0.15 ml). The reaction mixture was heated to 40° C. for 4 hours and then stored at ambient temperature of 16 hours. The reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml). The phases were separated. The aqueous layer was extracted with ethyl acetate. The combined organic extracts were concentrated. The residue was triturated with iso-hexane and dried under vacuum to give Compound No. B3 of Table B (408 mg) as a yellow solid.

後処理

  1. additionTo a suspension of Compound No
  2. customThe reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml)
  3. customThe phases were separated
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. concentrationThe combined organic extracts were concentrated
  6. customThe residue was triturated with iso-hexane
  7. customdried under vacuum
  8. customto give Compound No

出典と根拠

ORDレコード
ord-f719d410aef34e9fb96655d53d181f2b
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08133849B2

反応ノート

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