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Dichloromethane → (2-Butyl-4-chloro-1-((2'-(1-trityl-1H-tetraazol-5-YL)(1,1'-biphenyl)-4-YL)methyl)-1H-imidazol-5-YL)methanol

HRID 653938
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HRID 653938 반응식
C[Sn]([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:16]2[CH:21]=[CH:20][C:19]([CH2:22][N:23]3[C:27]([CH2:28][OH:29])=[C:26]([Cl:30])[N:25]=[C:24]3[CH2:31][CH2:32][CH2:33][CH3:34])=[CH:18][CH:17]=2)=[N:8][N:7]=[N:6]1)(C)C.C(Cl)Cl.[OH-].[Na+].[C:40]1([C:46](Cl)([C:53]2[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=2)[C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>O.O1CCCC1>[C:40]1([C:46]([N:5]2[C:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:16]3[CH:21]=[CH:20][C:19]([CH2:22][N:23]4[C:27]([CH2:28][OH:29])=[C:26]([Cl:30])[N:25]=[C:24]4[CH2:31][CH2:32][CH2:33][CH3:34])=[CH:18][CH:17]=3)=[N:8][N:7]=[N:6]2)([C:47]2[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=2)[C:53]2[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=2)[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 6456Trityl chloride2회HCID 14798Sodium Hydroxide3회HCID 144256651-[(2'-(Trimethylstannyltetrazol-5-yl)biphenyl-4-yl)methyl]-2-butyl-4-chloro-5-hydroxymethylimidazole

생성물 1

HCID 11643218(2-Butyl-4-chloro-1-((2'-(1-trityl-1H-tetraazol-5-YL)(1,1'-biphenyl)-4-YL)methyl)-1H-imidazol-5-YL)methanol

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

1-[(2'-(Trimethylstannyltetrazol-5-yl)-biphenyl-4-yl)methyl]-2-butyl-4-chloro-5-hydroxymethylimidazole (1.046 Kg), methylene chloride (5.00 L), tetrahydrofuran (0.85 L) and 10 N sodium hydroxide (192 ml) were charged to a 12 liter round-bottomed flask equipped with mechanical stirrer, condenser with N2 inlet, and thermometer. After stirring five minutes at room temperature, triphenylmethyl chloride (0.530 Kg) was added and the mixture stirred three hours. 10 N Sodium hydroxide (20 ml) and additional triphenylmethyl chloride (50 g) were added and the mixture stirred overnight. Deionized (D.I.) water (3.70 L) and 10 N sodium hydroxide (30 ml) were added and the phases allowed to separate. The organic phase was washed twice with 2.0 L portions of water, dried with sodium sulfate (100 g) and filtered into a 12 L round-bottomed flask equipped for distillation. Methylene chloride (~2.0 L) was distilled. Heating was discontinued and heptane (5.0 L) was added. The resulting slurry was stirred at ambient temperature over the weekend (18 68 hours). The mixture was cooled to ~5° C. and the product isolated by vacuum filtration, washed with heptane (1.0 L) and dried 48 hours in in vacuo at 40°-50° C. Yield: 959.5 g, 80%, M.P.: 167°-169° C. Purity by HPLC: 99.8%.

후처리

  1. customequipped with mechanical stirrer, condenser with N2 inlet
  2. stirringthe mixture stirred three hours
  3. stirringthe mixture stirred overnight
  4. customto separate
  5. washThe organic phase was washed twice with 2.0 L portions of water
  6. dry with materialdried with sodium sulfate (100 g)
  7. filtrationfiltered into a 12 L round-bottomed flask
  8. customequipped for distillation
  9. distillationMethylene chloride (~2.0 L) was distilled
  10. temperatureHeating
  11. additionheptane (5.0 L) was added
  12. stirringThe resulting slurry was stirred at ambient temperature over the weekend (18 68 hours)
  13. temperatureThe mixture was cooled to ~5° C.
  14. customthe product isolated by vacuum filtration
  15. washwashed with heptane (1.0 L)
  16. customdried 48 hours in in vacuo at 40°-50° C

출처 및 근거

ORD 기록
ord-7c5248a3d144444ea0ffd9da0e8b1851
출처 데이터셋
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05128355

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