Hydrochloric Acid → HCID 66701057、化合物

HRID 1643435ノート

反応式

HRID 1643435 の反応式
[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:25][CH2:24][C:11]3([CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[ClH:1].[ClH:1].[N:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:25][CH2:24][C:11]3([CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=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, the residue taken up in ethanol (3 ml) and the mixture cooled. Acetone (80 ml) was added and the mixture was stirred in an ice bath for 30 min. The precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo.

後処理

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. temperaturethe mixture cooled
  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-8e634edeb8a440f895568ee0659e5ba6
出典データセット
uspto-grants-2012_02
特許番号
US08119805B2

反応ノート

読み込み中…