Methanesulfonic Acid → 2-(4-Carboxypiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline methanesulfonate

HRID 1384916

反応式

HRID 1384916 の反応式
[C:1]([CH:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]([NH:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]4[O:28][CH2:29][O:30][C:24]=4[CH:23]=3)[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([Cl:31])[CH:16]=3)[N:11]=2)[CH2:6][CH2:5]1)([OH:3])=[O:2].[CH3:32][S:33]([OH:36])(=[O:35])=[O:34]>O1CCCC1.C(O)C>[CH3:32][S:33]([OH:36])(=[O:35])=[O:34].[C:1]([CH:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]([NH:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]4[O:28][CH2:29][O:30][C:24]=4[CH:23]=3)[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([Cl:31])[CH:16]=3)[N:11]=2)[CH2:6][CH2:5]1)([OH:3])=[O:2]

参加物

5

反応物 2

HCID 6395Methanesulfonic AcidHCID 53114861-(6-Chloro-4-(3,4-methylenedioxybenzyl)aminoquinazolin-2-yl)piperidine-4-carboxylic acid

生成物 1

HCID 211840322-(4-Carboxypiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline methanesulfonate収率 90.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

2.00 g (4.54 mmol) of the 2-(4-carboxypiperidino)-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline prepared in Example 222 was dissolved in a mixture comprising 25 ml of tetrahydrofuran and 25 ml of ethanol under heating, followed by the dropwise addition of 0.31 ml (4.78 mmol) of methanesulfonic acid. The obtained mixture was cooled by allowing to stand to precipitate crystals. The crystals were recovered by filtration, washed with tetrahydrofuran, and air-dried to give 2.21 g of the title compound.

後処理

  1. temperatureunder heating
  2. temperatureThe obtained mixture was cooled
  3. customto precipitate crystals
  4. filtrationThe crystals were recovered by filtration
  5. washwashed with tetrahydrofuran
  6. customair-dried

出典と根拠

ORDレコード
ord-ccd70cb7b8d64cc38ada2855e45ebce3
出典データセット
uspto-grants-2001_07
特許番号
US06262059B1

関連ノート

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