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Triethylamine → (+/-)-N-[2,6-Bis(1-methylethyl)phenyl]-2-dodecyl-alpha-fluoro-alpha-phenyl-2H-tetrazole-5-acetamide

HRID 1756920
ノート
印刷プレビュー

反応式

HRID 1756920 の反応式
C(Cl)(=O)C(Cl)=O.[CH2:7]([N:19]1[N:23]=[N:22][C:21]([C:24]([F:34])([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:25]([OH:27])=O)=[N:20]1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[CH:35]([C:38]1[CH:44]=[CH:43][CH:42]=[C:41]([CH:45]([CH3:47])[CH3:46])[C:39]=1[NH2:40])([CH3:37])[CH3:36].CCN(CC)CC>C(Cl)Cl.CN(C=O)C>[CH3:47][CH:45]([C:41]1[CH:42]=[CH:43][CH:44]=[C:38]([CH:35]([CH3:37])[CH3:36])[C:39]=1[NH:40][C:25](=[O:27])[C:24]([F:34])([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:21]1[N:22]=[N:23][N:19]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:20]=1)[CH3:46]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 65578Oxalyl chlorideHCID 539372962-Dodecyl-alpha-fluoro-alpha-phenyl-2H-tetrazole-5-acetic acid

生成物 1

HCID 9807593(+/-)-N-[2,6-Bis(1-methylethyl)phenyl]-2-dodecyl-alpha-fluoro-alpha-phenyl-2H-tetrazole-5-acetamide収率 0%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
触媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Oxalyl chloride (0.08 mL, 0.92 mmole) was added to a stirred solution of 2-dodecyl-α-fluoro-α-phenyl-2H-tetrazole-5-acetic acid (0.24 g, 0.61 mole) in 5 mL of CH2Cl2 at room temperature. The mixture was stirred 60 minutes, the one drop of DMF was added (immediate gas evolution). The solution was stirred overnight, concentrated (rotovap), toluene was added, and the solution concentrated again. The residue was dissolved in CH2Cl2 (3 mL) and added to a stirred solution of 2,6-diisopropylaniline (0.12 mL, 0.61 mole) and Et3N (0.14 mL, 1.0 mole) in CH2Cl2 (2 mL) cooled to 0° C. under dry nitrogen. After 20 minutes, the ice bath was removed and the solution allowed to warm to room temperature and stirred for 3 days. The mixture was then diluted with ethyl acetate (150 mL) and washed with dilute HCl (50 mL), bicarbonate (50 mL), brine (50 mL), and dried. Filtration and concentration afforded an oil which was flash chromatographed (silica gel, 10: 1 hexanes-ethyl acetate) to produce 150 mg of the title compound as an oil which solidified on standing.

後処理

  1. stirringThe solution was stirred overnight
  2. concentrationconcentrated (rotovap), toluene
  3. additionwas added
  4. concentrationthe solution concentrated again
  5. dissolutionThe residue was dissolved in CH2Cl2 (3 mL)
  6. waitAfter 20 minutes
  7. customthe ice bath was removed
  8. temperatureto warm to room temperature
  9. stirringstirred for 3 days
  10. additionThe mixture was then diluted with ethyl acetate (150 mL)
  11. washwashed with dilute HCl (50 mL), bicarbonate (50 mL), brine (50 mL)
  12. customdried
  13. filtrationFiltration and concentration
  14. customafforded an oil which
  15. customchromatographed (silica gel, 10: 1 hexanes-ethyl acetate)

出典と根拠

ORDレコード
ord-87dabbfd419541988361e53a28615706
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05441975

反応ノート

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