Hydrochloric Acid → HCID 66701057, 화합물

HRID 1808353노트

반응식

HRID 1808353 반응식
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][C:12]2([CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=3)[CH2:16][CH2:15]2)[CH2:11][CH2:10]1)=O)(C)(C)C>CO>[ClH:1].[ClH:1].[N:23]1[CH:22]=[CH:21][C:20]([N:17]2[CH2:18][CH2:19][C:12]3([CH2:13][CH2:14][NH:9][CH2:10][CH2:11]3)[CH2:15][CH2:16]2)=[CH:25][CH:24]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59486425tert-Butyl 9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carboxylate

생성물 1

HCID 66701057HCID 66701057, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Hydrogen chloride in methanol (1.25 mol/l, 6.3 ml) was added to tert-butyl-9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carboxylate (0.52 g, 1.569 mmol), and the mixture was refluxed for 1 h. The solvent was removed in vacuo, and the residue was taken up in ethanol (3 ml) and cooled. Acetone (80 ml) was added and stirring was carried out for 30 min. in an ice bath. The precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo. Yield: 0.4 g (83%) Alternatively, the deprotection can also be carried out under the action of TFA in DCM in order to obtain the amine (F-09) in the form of the free base.

후처리

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. temperaturecooled
  4. additionAcetone (80 ml) was added
  5. filtrationThe precipitate was filtered out with suction
  6. washwashed with diethyl ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-2837bc3976194ea58b40e907ea7e24aa
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357717B2

반응 노트

불러오는 중…