Methane → HCID 178456073, 화합물

HRID 865671

반응식

HRID 865671 반응식
[C:1]([N:3]=[C:4](OC1C=CC=CC=1)[NH:5][C:6]1[CH:7]=[N:8][C:9]([N:12]([CH3:14])[CH3:13])=[CH:10][CH:11]=1)#[N:2].[C:22]1([C@H:28]([NH2:31])[CH2:29][CH3:30])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.CN1CCOCC1.C>C(O)(C)C>[C:1]([N:3]=[C:4]([NH:31][C@@H:28]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH2:29][CH3:30])[NH:5][C:6]1[CH:7]=[N:8][C:9]([N:12]([CH3:13])[CH3:14])=[CH:10][CH:11]=1)#[N:2]

참가 물질

6

반응물 4

HCID 297MethaneHCID 79724-MethylmorpholineHCID 5324978(R)-1-PhenylpropylamineHCID 178482865HCID 178482865, 화합물

생성물 1

HCID 178456073HCID 178456073, 화합물수율 5.2%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A stirred solution of the product from Step 4 (2.00 g, 0.00711 mol), (R)-(+)-1-phenylpropylamine (1.06 g, 0.00784 mol), N-methylmorpholine (1.69 ml, 0.0154 mol) and isopropanol (13.3 ml) was refluxed, under nitrogen, until the reaction was shown to be complete by TLC (28 hours). It was then concentrated and the residue chromatographed on silica gel with 1 to 4% MeOH-CHCl3. A solution of the product thus obtained in MeOH-EtOAc was decolorized with Darco (activated charcoal) and crystallized from EtOAc-hexane to give 1.02 g, m.p. 109°-111° C. and 0.120 g, m.p. 107°-113° C. of the titled product.

후처리

  1. customto be complete by TLC (28 hours)
  2. concentrationIt was then concentrated
  3. customthe residue chromatographed on silica gel with 1 to 4% MeOH-CHCl3
  4. customA solution of the product thus obtained in MeOH-EtOAc
  5. customcrystallized from EtOAc-hexane

출처 및 근거

ORD 기록
ord-305b6d1802174bafaad6803f6180f433
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05567722

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