Oxalyl chloride → HCID 71556276、化合物

HRID 929489ノート

反応式

HRID 929489 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[C:10](O)[C:9]2=[O:21])=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:25])=O>CN(C=O)C>[Cl:25][C:10]1[C:9](=[O:21])[N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:12](=[O:13])[C:11]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 86709896HCID 86709896、化合物

生成物 1

HCID 71556276HCID 71556276、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

After dissolving compound 6d (1.00 g, 3.33 mmol) in MC (10 ml) and anhydrous DMF (10 ml), oxalyl chloride (0.850 g, 6.66 mmoL) was added thereto and the agitation for 30 minutes was carried out. After the identification of the reaction progress with TLC, the reaction was terminated. Then, three times extractions were carried out with EA and three times washings were carried out with brine. Water was removed by using Na2SO4, solvents were removed and then, the column chromatography was carried out with EA/HX ( 1/15). The suspension was carried out with HX to obtain compound 7d.

後処理

  1. additionwas added
  2. customAfter the identification of the reaction progress with TLC, the reaction was terminated
  3. extractionThen, three times extractions
  4. customWater was removed
  5. customwere removed

出典と根拠

ORDレコード
ord-9a277de1c5bf4ac781df43b75492ee22
出典データセット
uspto-grants-2016_03
特許番号
US09296690B2

反応ノート

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