Hydrochloric Acid → 1-{4-[(2H-1,3-benzodioxol-5-ylmethyl)amino]-6-chloroquinazolin-2-yl}piperidine-4-carboxylic acid hydrochloride

HRID 1900692

反応式

HRID 1900692 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].Cl>O1CCCC1.C(O)C>[ClH:31].[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 313Hydrochloric AcidHCID 53114861-(6-Chloro-4-(3,4-methylenedioxybenzyl)aminoquinazolin-2-yl)piperidine-4-carboxylic acid

生成物 1

HCID 211839871-{4-[(2H-1,3-benzodioxol-5-ylmethyl)amino]-6-chloroquinazolin-2-yl}piperidine-4-carboxylic acid hydrochloride収率 172.6%

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-carboxy-piperidino)-4-(3,4-methylenedioxybenzylamino)-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 1.0 ml of an 8M ethanolic solution of hydrochloric 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 1.87 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-d0e4aa5a3f75414bb53fa265afda8f3d
出典データセット
uspto-grants-1996_11
特許番号
US05576322

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