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1-Hydroxybenzotriazole → HCID 58243385, 화합물

HRID 2361686
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HRID 2361686 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][N:3]=1.C1C=CC2N(O)N=NC=2C=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:45]1([N:49]2[CH2:55][CH2:54][CH2:53][N:52]([C:56]([N:58]3[CH2:61][CH:60]([NH2:62])[CH2:59]3)=[O:57])[CH2:51][CH2:50]2)[CH2:48][CH2:47][CH2:46]1>CN(C=O)C.C(Cl)Cl>[CH:45]1([N:49]2[CH2:55][CH2:54][CH2:53][N:52]([C:56]([N:58]3[CH2:59][CH:60]([NH:62][C:6]([C:5]4[CH:4]=[N:3][C:2]([CH3:1])=[CH:10][CH:9]=4)=[O:8])[CH2:61]3)=[O:57])[CH2:51][CH2:50]2)[CH2:48][CH2:47][CH2:46]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 1378606-Methylnicotinic acidHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 44477248HCID 44477248, 화합물

생성물 1

HCID 58243385HCID 58243385, 화합물수율 34%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 6-methylnicotinic acid (5.5 mg, 40 μmol) in 1:1 DCM:DMF (1 ml) was added HOBt (12 mg, 87 μmol) followed by HBTU (30 mg, 80 μmol) at room temperature. After 15 minutes 1-[(4-cyclobutyl-1,4-diazepan-1-yl)carbonyl]azetidin-3-amine (10 mg, 40 μmol) was added and the reaction was stirred for 16 hours. The reaction was concentrated at reduced pressure and purified directly via preparative HPLC to give the title compound (5 mg, 34%).

후처리

  1. concentrationThe reaction was concentrated at reduced pressure
  2. custompurified directly via preparative HPLC

출처 및 근거

ORD 기록
ord-daa36e2fed834ff49d5e76fec3a7433f
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691804B2

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