Sodium Carbonate → HCID 178496013、化合物

HRID 75529ノート

反応式

HRID 75529 の反応式
[C:1]([NH:3][C@@H:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C@@H:5]1[NH:10][C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([CH3:21])[CH:19]=2)[N:14]=[C:13]([C:22]([NH:24][CH2:25][CH2:26][O:27][CH3:28])=[O:23])[N:12]=1)#[N:2].Cl.[CH3:30][O:31][NH2:32].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[NH2:2][C:1]([NH:3][C@@H:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C@@H:5]1[NH:10][C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([CH3:21])[CH:19]=2)[N:14]=[C:13]([C:22]([NH:24][CH2:25][CH2:26][O:27][CH3:28])=[O:23])[N:12]=1)=[N:32][O:31][CH3:30]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 866384014-{[(1S,2R)-2-(cyanoamino)cyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide

生成物 1

HCID 178496013HCID 178496013、化合物収率 77.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.96 g of 4-{[(1S,2R)-2-(cyanoamino)cyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide and 8.56 g of methoxyamine hydrochloride in 80 ml of ethanol, 10.86 g of sodium carbonate was added and the mixture was heated at reflux for 1 hour. The reaction solution was added to 400 ml of ice water, and the deposited substance was collected by filtration. After the collected deposited substance was washed with water, it was dried under reduced pressure. The obtained powder was washed with a mixed solution of (chloroform:diisopropyl alcohol=1:1), whereby 1.71 g of a desired compound was obtained as a white powder.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 hour
  3. filtrationthe deposited substance was collected by filtration
  4. washAfter the collected deposited substance was washed with water, it
  5. customwas dried under reduced pressure
  6. washThe obtained powder was washed with a mixed solution of (chloroform:diisopropyl alcohol=1:1)

出典と根拠

ORDレコード
ord-31ac90c69935415cb725f33e43330a81
出典データセット
uspto-grants-2014_09
特許番号
US08835446B2

反応ノート

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