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

HRID 1384915

반응식

HRID 1384915 반응식
[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]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 53114861-(6-Chloro-4-(3,4-methylenedioxybenzyl)aminoquinazolin-2-yl)piperidine-4-carboxylic acid

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f9a4801271947a88f1e365eab659da6
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06262059B1

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