Hydrochloric Acid → (9-(Pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)(4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl)methanone hydrochloride

HRID 1808369ノート

反応式

HRID 1808369 の反応式
[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:36][CH2:35][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[S:27][C:26]5[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22][C:21]=5[CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:36][CH2:35][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[S:27][C:26]5[CH2:25][CH2:24][NH:23][CH2:22][C:21]=5[CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59483855HCID 59483855、化合物

生成物 1

HCID 68507109(9-(Pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)(4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl)methanone hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Hydrogen chloride in methanol (2.3 ml, 2.82 mmol, 1.25 mol/l) was added at room temperature to a solution of tert-butyl 2-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)-6,7-dihydrothieno[3,2-c]pyridine-5(4H)-carboxylate (280 mg, 0.564 mmol) in methanol (2 ml), and the reaction mixture was refluxed for 2 h. The solvent was removed in vacuo, the residue was taken up in a small amount of ethanol (3 ml), and diethyl ether (50 ml) was added thereto. Cooling was then carried out for 30 min. in an ice bath, and the resulting solid was filtered out, washed with diethyl ether and dried in vacuo. Yield: 180 mg (73%)

後処理

  1. temperaturethe reaction mixture was refluxed for 2 h
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureCooling
  5. filtrationthe resulting solid was filtered out
  6. washwashed with diethyl ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-c2f8bdfde81a497fa7a66590f9910aea
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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