Triethylamine → HCID 136404631, 화합물

HRID 613349노트

반응식

HRID 613349 반응식
Cl.[N:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([OH:16])=[O:15])[CH:6]=[CH:5][N:4]=[CH:3]1.C(N(CC)CC)C.O[CH2:25][C:26]1[CH:30]=[C:29]2[C:31]([C:89]3[CH:94]=[CH:93][CH:92]=[CH:91][C:90]=3[NH:95][C:96](=[O:101])[C:97]([CH3:100])([CH3:99])[CH3:98])=[C:32]3[N:36]=[C:35]([C:37]([C:76]4[CH:81]=[CH:80][CH:79]=[CH:78][C:77]=4[NH:82][C:83](=[O:88])[C:84]([CH3:87])([CH3:86])[CH3:85])=[C:38]4[NH:42][C:41](=[C:43]([C:63]5[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=5[NH:69][C:70](=[O:75])[C:71]([CH3:74])([CH3:73])[CH3:72])[C:44]5[CH:45]=[CH:46][C:47](=[C:49]([C:50]6[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=6[NH:56][C:57](=[O:62])[C:58]([CH3:61])([CH3:60])[CH3:59])[C:27]=1[NH:28]2)[N:48]=5)[CH:40]=[CH:39]4)[CH:34]=[CH:33]3.C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C.CN(C1C=CN=CC=1)C>[N:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:25][C:26]2[CH:30]=[C:29]3[C:31]([C:89]4[CH:94]=[CH:93][CH:92]=[CH:91][C:90]=4[NH:95][C:96](=[O:101])[C:97]([CH3:100])([CH3:99])[CH3:98])=[C:32]4[N:36]=[C:35]([C:37]([C:76]5[CH:81]=[CH:80][CH:79]=[CH:78][C:77]=5[NH:82][C:83](=[O:88])[C:84]([CH3:87])([CH3:85])[CH3:86])=[C:38]5[NH:42][C:41](=[C:43]([C:63]6[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=6[NH:69][C:70](=[O:75])[C:71]([CH3:72])([CH3:73])[CH3:74])[C:44]6[CH:45]=[CH:46][C:47](=[C:49]([C:50]7[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=7[NH:56][C:57](=[O:62])[C:58]([CH3:59])([CH3:60])[CH3:61])[C:27]=2[NH:28]3)[N:48]=6)[CH:40]=[CH:39]5)[CH:34]=[CH:33]4)=[O:15])[CH:6]=[CH:5][N:4]=[CH:3]1

참가 물질

7

반응물 4

HCID 8471Triethylamine2회HCID 10868DicyclohexylcarbodiimideHCID 12870425HCID 12870425, 화합물HCID 136404630HCID 136404630, 화합물

생성물 1

HCID 136404631HCID 136404631, 화합물수율 89%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

8-Imidazol-1-yloctanoic acid hydrochloride (90.1 mg, 0.37 mmol) and triethylamine (TEA, 0.1 ml, 0.74 mmol) were dissolved in dry DMF (4 ml) and stirred for 10 min. After removing TEA under reduced pressure, 2-hydroxymethyl-5,10,15,20-tetrakis(o-pivalamidophenyl)porphyrin, 76 mg, 73 μmol), 4-(N,N-dimethylamino)pyridine (DMAP, 4.5 mg, 37 μmol) and dicyclohexylcarbodiimide (DCC, 75.4 mg, 0.37 mmol) were added to the solution and stirred for 84 hours at room temperature in darkness. The mixture was chromatographed on a silica gel flash column using CHCl3 --MeOH (30/1 v/v) as the eluent. The residue was dried at room temperature in vacuo to give a purple product, 2-(8-imidazol-1-yloctanoyloxymethyl)-5,10,15,20-tetrakis(o-pivalamidophenyl)porphyrin (80 mg, 89%).

후처리

  1. additionwere added to the solution
  2. stirringstirred for 84 hours at room temperature in darkness
  3. customThe mixture was chromatographed on a silica gel flash column
  4. customThe residue was dried at room temperature in vacuo

출처 및 근거

ORD 기록
ord-be0803a4a1f34b0198d2786248d524a6
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06008198

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