4-Methylmorpholine → HCID 178508775, 화합물

HRID 1665121노트

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HRID 1665121 반응식
Cl.Cl.[NH:3]1[C:7]2([CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH2:6][NH:5]/[C:4]/1=[N:13]\[C:14]([C:16]1[C:21]([NH2:22])=[N:20][C:19]([NH2:23])=[C:18]([Cl:24])[N:17]=1)=[O:15].[CH2:25]([O:32][C:33]1[CH:38]=[CH:37][C:36]([CH2:39][C:40](O)=[O:41])=[CH:35][CH:34]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.CN1CCOCC1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(Cl)Cl>[CH2:25]([O:32][C:33]1[CH:34]=[CH:35][C:36]([CH2:39][C:40]([N:10]2[CH2:9][CH2:8][C:7]3([NH:3]/[C:4](=[N:13]/[C:14]([C:16]4[C:21]([NH2:22])=[N:20][C:19]([NH2:23])=[C:18]([Cl:24])[N:17]=4)=[O:15])/[NH:5][CH2:6]3)[CH2:12][CH2:11]2)=[O:41])=[CH:37][CH:38]=1)[C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

7

반응물 4

HCID 79724-MethylmorpholineHCID 810334-Benzyloxyphenylacetic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178478673HCID 178478673, 화합물

생성물 1

HCID 178508775HCID 178508775, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 3,5-diamino-6-chloro-pyrazine-2-carboxylic acid [1,3,8-triaza-spiro[4.5]dec-(2E)-ylidene]-amide dihydrochloride (Ex. 38) (300 mg, 0.83 mmol), 4-benzyloxyphenylacetic acid (200 mg, 0.83 mmol), N-methyl morpholine (0.40 ml, 3.64 mmol) and HATU (315 mg, 0.83 mmol) in anhydrous DMF (20 ml) is stirred at room temperature for 16 hours. The reaction mixture is concentrated in vacuo and subjected to column chromatography (basic alumina, 0-3% MeOH in DCM) to obtain pale yellow solid. The product is dissolved in DCM and MeOH and re-precipitated by adding diethyl ether. The supernatant solvent mixture is decanted and the product is washed again with diethyl ether and dried under vacuum to afford the title compound as a pale yellow solid; [M+H]+ 549.

후처리

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. customto obtain pale yellow solid
  3. customMeOH and re-precipitated
  4. additionby adding diethyl ether
  5. customThe supernatant solvent mixture is decanted
  6. washthe product is washed again with diethyl ether
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-abf193bd515c4c2ab52b1abcaf61f02a
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039472B2

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