Oxalyl chloride → HCID 23293589、化合物

HRID 1954900ノート

反応式

HRID 1954900 の反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([CH3:16])([CH3:15])[CH2:7]/[C:8]/2=[CH:11]\[C:12](O)=[O:13])=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:20])=O>ClCCl>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([CH3:16])([CH3:15])[CH2:7]/[C:8]/2=[CH:11]\[C:12]([Cl:20])=[O:13])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 23293609Acetic acid, (6-fluoro-2,3-dihydro-3,3-dimethyl-1H-inden-1-ylidene)-, (2E)-

生成物 1

HCID 23293589HCID 23293589、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

To an ice cold, stirred suspension of (E)-2-(6-fluoro-3,3-dimethyl-1-indanylidene)acetic acid (9.0 g, 0.0409 mol) in dichloromethane (200 ml) was added oxalyl chloride (15.6 g, 0.123 mol, Aldrich). The stirring suspension was allowed to warm to 25° C. during 2 h. The resulting solution was concentrated by spin evaporation in vacuo with the addition of dichloromethane (4×75 ml) to give (E)-2-(6-fluoro-3,3-dimethyl-1-indanylidene)acetyl chloride as an uncharacterized oil. Dichloromethane (approximately 70 g) was added to dissolve this residual oil and the resulting solution was divided equally and used without other purification in Examples 15i, 16 and 17.

後処理

  1. concentrationThe resulting solution was concentrated by spin evaporation in vacuo with the addition of dichloromethane (4×75 ml)

出典と根拠

ORDレコード
ord-ad57b52361464173af6b0ab894caef4a
出典データセット
uspto-grants-2000_09
特許番号
US06124284

反応ノート

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