Oxalyl chloride → 3,3-Bis(4-fluorophenyl)-2-[1-(1-methylethyl)-1H-tetrazol-5-yl]-2-propenolchloride

HRID 974456ノート

反応式

HRID 974456 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)=[C:9]([C:13]2[N:17]([CH:18]([CH3:20])[CH3:19])[N:16]=[N:15][N:14]=2)[C:10](O)=[O:11])=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:31])=O>C(Cl)Cl>[Cl-:31].[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)=[C:9]([C:13]2[N:17]([CH:18]([CH3:20])[CH3:19])[N:16]=[N:15][N:14]=2)[CH2:10][OH:11])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 147238703,3-Bis(4-fluorophenyl)-2-[1-(1-methylethyl)-1H-tetrazol-5-yl]-2-propenoic acid

生成物 1

HCID 199862413,3-Bis(4-fluorophenyl)-2-[1-(1-methylethyl)-1H-tetrazol-5-yl]-2-propenolchloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of the dried acid prepared in Step A in 20 mL of dry methylene chloride at room temperature was treated with 4 mL of oxalyl chloride (redistilled over CaH2). The mixture was refluxed under an argon atmosphere for two hours forming a light brownish solution. Most of the volatile solvents were evaporated under reduced pressure and the last traces of oxalyl choride were removed under high vacuum (0.01 mmHg) at room temperature for 12 hours to give the title compound.

後処理

  1. temperatureThe mixture was refluxed under an argon atmosphere for two hours
  2. customforming a light brownish solution
  3. customMost of the volatile solvents were evaporated under reduced pressure
  4. customthe last traces of oxalyl choride were removed under high vacuum (0.01 mmHg) at room temperature for 12 hours

出典と根拠

ORDレコード
ord-ce44c8b4027e4bb8b631cc27a8a4d451
出典データセット
uspto-grants-1991_11
特許番号
US05068346

反応ノート

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