Hydrochloric Acid → HCID 66701057、化合物

HRID 1808353ノート

反応式

HRID 1808353 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 66701057HCID 66701057、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2837bc3976194ea58b40e907ea7e24aa
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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