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Morpholine → HCID 178481612, 화합물

HRID 538058
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HRID 538058 반응식
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([F:14])([F:13])[F:12])=[CH:10][C:5]=2[N:4]([CH2:15][C@H:16]2[CH2:21][CH2:20][C@H:19]([C:22](O)=[O:23])[CH2:18][CH2:17]2)[C:3]1=[O:25].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH:50]1[CH2:55][CH2:54][O:53][CH2:52][CH2:51]1.C(N(CC)CC)C.[Cl-].[NH4+]>CS(C)=O.C(Cl)Cl>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([F:12])([F:14])[F:13])=[CH:10][C:5]=2[N:4]([CH2:15][C@H:16]2[CH2:21][CH2:20][C@H:19]([C:22]([N:50]3[CH2:55][CH2:54][O:53][CH2:52][CH2:51]3)=[O:23])[CH2:18][CH2:17]2)[C:3]1=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 8083MorpholineHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178481613HCID 178481613, 화합물

생성물 1

HCID 178481612HCID 178481612, 화합물
수율 27%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매

실험 절차

trans-4-(3-Methyl-2-oxo-6-trifluoromethyl-2,3-dihydro-benzoimidazol-1-ylmethyl)cyclohexanecarboxylic acid (78 mg, 0.22 mmol), HATU (100 mg, 0.26 mmol), morpholine (23 mg, 0.26 mmol) and triethyl amine (0.04 ml, 0.26 mmol) were dissolved in DMSO and the mixture were shaken overnight. 3 ml of a saturated solution of ammonium chloride and 2 ml of DCM were added and the organic layer was separated and washed with water. The organic solvent was evaporated and the crude was purified by silica column using ethyl acetate as eluent. 25 mg (yield 27%) of the titled compound were isolated.

후처리

  1. customthe organic layer was separated
  2. washwashed with water
  3. customThe organic solvent was evaporated
  4. customthe crude was purified by silica column

출처 및 근거

ORD 기록
ord-bdc7b1a0597d4ed792a9ba8a01fbadd4
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865704B2

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