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

HRID 1195334노트

반응식

HRID 1195334 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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 chloride were removed under high vacuum (0.01 mmHg) at room temperature for 12 hours to give the title compound.

후처리

  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 chloride were removed under high vacuum (0.01 mmHg) at room temperature for 12 hours

출처 및 근거

ORD 기록
ord-5e999b48694645488369c4ceb7009d85
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05110940

반응 노트

불러오는 중…