Ammonium Chloride → N-[1-(2-phenylethyl)-5-chloro-4-ethoxycarbonylpyrazol-3-yl]-N-[(2'-(N-triphenylmethyl-(1H-tetrazol-5-yl))-biphenyl-4-yl)methyl]-n-propylamine

HRID 357903노트

반응식

HRID 357903 반응식
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].CCCC[CH2:10][CH3:11].C1([CH2:18][CH2:19][N:20]2[C:24](Br)=[C:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[C:22]([N:31]([CH2:69][CH2:70][CH3:71])[CH2:32][C:33]3[CH:38]=[CH:37][C:36]([C:39]4[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=4[C:45]4[N:49]([C:50]([C:63]5[CH:68]=[CH:67][CH:66]=[CH:65][CH:64]=5)([C:57]5[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=5)[C:51]5[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=5)[N:48]=[N:47][N:46]=4)=[CH:35][CH:34]=3)=[N:21]2)C=CC=CC=1.C(=O)=O.CC(C)=O.[Cl:79]N1C(=O)CCC1=O.[Cl-].[NH4+]>C1COCC1>[C:4]1([CH2:18][CH2:19][N:20]2[C:24]([Cl:79])=[C:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[C:22]([N:31]([CH2:69][CH2:70][CH3:71])[CH2:32][C:33]3[CH:34]=[CH:35][C:36]([C:39]4[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=4[C:45]4[N:49]([C:50]([C:51]5[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=5)([C:57]5[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=5)[C:63]5[CH:64]=[CH:65][CH:66]=[CH:67][CH:68]=5)[N:48]=[N:47][N:46]=4)=[CH:37][CH:38]=3)=[N:21]2)[CH:11]=[CH:10][CH:1]=[CH:2][CH:3]=1

참가 물질

7

반응물 5

HCID 25517Ammonium ChlorideHCID 31398ChlorosuccinimideHCID 18522661Acetone cardiceHCID 22103828N-[1-(2-phenylethyl)-4-ethoxycarbonyl-5-bromopyrazol-3-yl]-N-[(2'-(N-triphenylmethyl-(1H-tetrazol-5-yl))biphenyl-4-yl)methyl]-n-propylamineHCID 178418244HCID 178418244, 화합물

생성물 1

HCID 22103835N-[1-(2-phenylethyl)-5-chloro-4-ethoxycarbonylpyrazol-3-yl]-N-[(2'-(N-triphenylmethyl-(1H-tetrazol-5-yl))-biphenyl-4-yl)methyl]-n-propylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

0.24 ml of 1.6M n-butyl lithium/hexane solution were added to THF solution (10 ml) of 231 mg of N-[1-(2-phenylethyl)-5-bromo-4-ethoxycarbonylpyrazol-3-yl]-N-[(2'-(N-triphenylmethyl-(1H-tetrazol-5-yl))biphenyl-4-yl)methyl]-n-propylamine, while cooling with dry ice-acetone. After stirred for 30 minutes, 49 mg of N-chlorosuccinimide were added thereto and stirred for 30 minutes. 10 ml of aqueous ammonium chloride solution were added to the reaction solution, THF was distilled off under reduced pressure, and the resultant was extracted with 50 ml of dichloromethane. After dried over magnesium sulfate, the resultant was subjected to silica gel column chromatography (n-hexane-ethyl acetate=5:1) to obtain 159 mg of the intended compound as a pale yellow, amorphous solid.

후처리

  1. stirringstirred for 30 minutes
  2. distillationwas distilled off under reduced pressure
  3. extractionthe resultant was extracted with 50 ml of dichloromethane
  4. dry with materialAfter dried over magnesium sulfate

출처 및 근거

ORD 기록
ord-61da680a30a1495c803342b5bdf0a78d
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840909

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