Formic Acid → HCID 90387472, 화합물

HRID 508402노트

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HRID 508402 반응식
[CH:1](O)=[O:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[NH2:37][C@H:38]([CH2:47][C:48]1[CH:53]=[CH:52][C:51]([C:54]2[CH:59]=[CH:58][CH:57]=[C:56]([Cl:60])[CH:55]=2)=[CH:50][CH:49]=1)[CH2:39][C@:40]([CH2:45][OH:46])([CH3:44])[C:41]([OH:43])=[O:42]>CN(C=O)C>[Cl:60][C:56]1[CH:55]=[C:54]([C:51]2[CH:52]=[CH:53][C:48]([CH2:47][C@@H:38]([NH:37][CH:1]=[O:2])[CH2:39][C@:40]([CH2:45][OH:46])([CH3:44])[C:41]([OH:43])=[O:42])=[CH:49][CH:50]=2)[CH:59]=[CH:58][CH:57]=1

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 81531Diisopropylethylamine2회HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 89964569HCID 89964569, 화합물

생성물 1

HCID 90387472HCID 90387472, 화합물수율 4.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Formic acid (3 mg, 32 μmol) was combined with HATU (12 mg, 32 μmol) and DMF (0.2 mL) and stirred for 5 minutes. DIPEA (17 μl, 96 μmol) was added, followed by (2S,4R)-4-amino-5-(3′-chlorobiphenyl-4-yl)-2-hydroxymethyl-2-methyl-pentanoic acid (79 mg, 38 μmol) pre-dissolved in DMF (0.5 mL) and DIPEA (17 μl, 96 μmol). The resulting mixture was stirred for 15 minutes. The solvent was removed in vacuo and the residue was dissolved in AcOH and purified by preparative HPLC to yield the title compound (0.5 mg). MS m/z [M+H]+ calc'd for C20H22ClNO4, 376.12. found 376.2.

후처리

  1. stirringThe resulting mixture was stirred for 15 minutes
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in AcOH
  4. custompurified by preparative HPLC

출처 및 근거

ORD 기록
ord-ee8033c3377c4efe939b4c0cd7822a7d
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096496B2

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