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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Toluene → tert-Butyl (3S)-3-[({[6-chloro-2,4,8,18,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-yl]amino}carbonyl)amino]pyrrolidine-1-carboxylate

HRID 541761
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HRID 541761 반응식
C(Cl)(Cl)=O.C1(C)C=CC=CC=1.[NH2:12][C@H:13]1[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14]1.C(N(CC)CC)C.FC(F)(F)[C:34]([OH:36])=O.FC(F)(F)C(O)=O.[Cl:46][C:47]1[CH:48]=[N:49][C:50]2[NH:51][C:52]3[CH:53]=[N:54][CH:55]=[C:56]([CH:69]=3)[CH2:57][CH2:58][C:59]3[CH:67]=[C:63]([NH:64][C:65]=1[N:66]=2)[CH:62]=[CH:61][C:60]=3[NH2:68]>C1COCC1>[Cl:46][C:47]1[CH:48]=[N:49][C:50]2[NH:51][C:52]3[CH:53]=[N:54][CH:55]=[C:56]([CH:69]=3)[CH2:57][CH2:58][C:59]3[CH:67]=[C:63]([NH:64][C:65]=1[N:66]=2)[CH:62]=[CH:61][C:60]=3[NH:68][C:34]([NH:12][C@H:13]1[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14]1)=[O:36]
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참가 물질

7

반응물 5

HCID 1140TolueneHCID 6371PhosgeneHCID 8471Triethylamine2회HCID 854071tert-butyl (3S)-3-aminopyrrolidine-1-carboxylateHCID 866361696-Chloro-2,4,8,18,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine bis(trifluoroacetate)

생성물 1

HCID 57961783
tert-Butyl (3S)-3-[({[6-chloro-2,4,8,18,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-yl]amino}carbonyl)amino]pyrrolidine-1-carboxylate
수율 61.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 20% phosgene in toluene (0.49 mL, 0.93 mmol) was added a solution of tert-butyl (3S)-3-aminopyrrolidine-1-carboxylate (38 mg, 0.20 mmol) and triethylamine (102 μL, 0.734 mmol) in THF (0.5 mL). The resulting solution was stirred for 2 hours then concentrated. To the isolated solids was added DCM (0.75 mL) followed by 6-chloro-2,4,8,18,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine bis(trifluoroacetate) (70 mg, 0.1 mmol) and triethylamine (73 μL, 0.52 mmol). The resulting mixture was stirred at room temperature overnight and concentrated. The residue was purified by flash column chromatography to yield the desired product (34 mg, 50%). LCMS calculated for C27H32ClN8O3(M+H)+: m/z=551.1.

후처리

  1. concentrationthen concentrated
  2. additionTo the isolated solids was added DCM (0.75 mL)
  3. stirringThe resulting mixture was stirred at room temperature overnight
  4. concentrationconcentrated
  5. customThe residue was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-e573a85c93f941d7bb6052b86e4ce5ae
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871753B2

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