4-Methylmorpholine → HCID 178427372, 화합물

HRID 1665126노트

반응식

HRID 1665126 반응식
[C:1]1([CH3:18])[CH:6]=[CH:5][C:4]([S:7]([N:10]2[CH:14]=[CH:13][C:12]([C:15]([OH:17])=O)=[CH:11]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1.N=C=N.Cl.Cl.[NH:24]1[C:28]2([CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)[CH2:27][NH:26]/[C:25]/1=[N:34]\[C:35]([C:37]1[C:42]([NH2:43])=[N:41][C:40]([NH2:44])=[C:39]([Cl:45])[N:38]=1)=[O:36].CN1CCOCC1>CN1C(=O)CCC1>[C:1]1([CH3:18])[CH:2]=[CH:3][C:4]([S:7]([N:10]2[CH:14]=[CH:13][C:12]([C:15]([N:31]3[CH2:32][CH2:33][C:28]4([NH:24]/[C:25](=[N:34]/[C:35]([C:37]5[C:42]([NH2:43])=[N:41][C:40]([NH2:44])=[C:39]([Cl:45])[N:38]=5)=[O:36])/[NH:26][CH2:27]4)[CH2:29][CH2:30]3)=[O:17])=[CH:11]2)(=[O:8])=[O:9])=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 160435CarbodiimideHCID 27246931-(4-methylbenzenesulfonyl)-1H-pyrrole-3-carboxylic acidHCID 178478673HCID 178478673, 화합물

생성물 1

HCID 178427372HCID 178427372, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매2회

실험 절차

A solution of 1-(Toluene-4-sulfonyl)-1H-pyrrole-3-carboxylic acid (0.023 g, 0.085 mmol) in NMP (850 □l) is added to PS-carbodiimide (190 mg of 1.3 mmol/g loading, 0.24 mmol), followed by a solution of 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid [1,3,8-triaza-spiro[4.5]dec-(2E)-ylidene]-amide dihydrochloride (Ex. 38) (0.08 mmol) and N-methyl morpholine (8 □l, 0.08 mmol) in NMP (1 ml), and the resulting reaction mixture is shaken at room temperature. The reaction mixture is filtered and the resin is washed with NMP (1 ml). The collected filtrate is concentrated in vacuo and the residues are purified by mass-directed preparative HPLC. The purified fractions are evaporated under vacuum to afford the title compound; [M+H]+ 572.08

후처리

  1. customthe resulting reaction mixture
  2. filtrationThe reaction mixture is filtered
  3. washthe resin is washed with NMP (1 ml)
  4. concentrationThe collected filtrate is concentrated in vacuo
  5. customthe residues are purified by mass-directed preparative HPLC
  6. customThe purified fractions are evaporated under vacuum

출처 및 근거

ORD 기록
ord-f1de0c0c2c7444218adc86902f7ecc23
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039472B2

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