Oxalyl chloride → HCID 59625913、化合物

HRID 1023077ノート

反応式

HRID 1023077 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][CH:19]=1)[CH2:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11](O)=[O:12])=[CH:9][C:8]=1[Cl:16].C(Cl)(=O)C([Cl:23])=O>C1COCC1.CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][CH:19]=1)[CH2:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([Cl:23])=[O:12])=[CH:9][C:8]=1[Cl:16]

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 8707028HCID 8707028、化合物

生成物 1

HCID 59625913HCID 59625913、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of compound 27d (67 mg, 0.33 mmol) in THF (2 mL) was added oxalyl dichloride (43 μL, 0.50 mmol) dropwise at 0° C., followed by the addition of 2 drops of DMF. The resultant mixture was stirred at 0° C. for 3 h, and then was warmed up to room temperature over 18 h. The solvents were removed under reduced pressure. The resultant residue, crude compound 27e, was dried under reduced pressure for 2 h and used in the following step without further purification.

後処理

  1. customThe solvents were removed under reduced pressure
  2. dry with materialThe resultant residue, crude compound 27e, was dried under reduced pressure for 2 h
  3. customused in the following step without further purification

出典と根拠

ORDレコード
ord-96337ace49a8406eb5fb10e861a1bf26
出典データセット
uspto-grants-2014_05
特許番号
US08722658B2

反応ノート

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