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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Trifluoroacetic acid → (S)-(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)amine

HRID 507036
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HRID 507036 반응식
FC(F)(F)C(O)=O.[F:8][C:9]([F:52])([F:51])[C:10]1[CH:11]=[C:12]([CH:44]=[C:45]([C:47]([F:50])([F:49])[F:48])[CH:46]=1)[CH2:13][N:14]([C:38]1[N:39]=[N:40][N:41]([CH3:43])[N:42]=1)[C@H:15]1[CH2:21][CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[C:17]2[CH:29]=[C:30]([C:34]([F:37])([F:36])[F:35])[C:31]([CH3:33])=[CH:32][C:16]1=2.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[F:51][C:9]([F:8])([F:52])[C:10]1[CH:11]=[C:12]([CH:44]=[C:45]([C:47]([F:50])([F:48])[F:49])[CH:46]=1)[CH2:13][N:14]([C:38]1[N:39]=[N:40][N:41]([CH3:43])[N:42]=1)[C@H:15]1[CH2:21][CH2:20][CH2:19][NH:18][C:17]2[CH:29]=[C:30]([C:34]([F:35])([F:36])[F:37])[C:31]([CH3:33])=[CH:32][C:16]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 11585492(S)-tert-Butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate

생성물 1

HCID 59432408(S)-(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)amine수율 100.1%

시약·촉매·용매

1
HCID 6344Dichloromethane용매

실험 절차

Add trifluoroacetic acid (10 mL) to a solution of (S)-tert-butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (2.04 g, 3.13 mmol) in methylene chloride (50 mL) at 0° C. under nitrogen. Warm the mixture to room temperature, stir for 8 h and pour the mixture into saturated aqueous sodium bicarbonate solution (200 mL). Extract the mixture with methylene chloride (200 mL) and wash the combined organic extracts with brine (50 mL), dry over anhydrous sodium sulfate and filter. Remove the solvent under reduced pressure to provide the title compound as a colorless oil (1.73 g, >99%), which is used in the next step without purification. APCI MS m/z 553 (M+H)+.

후처리

  1. extractionExtract the mixture with methylene chloride (200 mL)
  2. washwash the combined organic extracts with brine (50 mL)
  3. dry with materialdry over anhydrous sodium sulfate
  4. filtrationfilter
  5. customRemove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-a5a407774c004243bc449609cc1ba51e
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786108B2

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