Methane → HCID 178456073、化合物

HRID 865671

反応式

HRID 865671 の反応式
[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]

参加物

6

反応物 4

HCID 297MethaneHCID 79724-MethylmorpholineHCID 5324978(R)-1-PhenylpropylamineHCID 178482865HCID 178482865、化合物

生成物 1

HCID 178456073HCID 178456073、化合物収率 5.2%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-305b6d1802174bafaad6803f6180f433
出典データセット
uspto-grants-1996_10
特許番号
US05567722

関連ノート

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