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 1808369노트

반응식

HRID 1808369 반응식
[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

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59483855HCID 59483855, 화합물

생성물 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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-c2f8bdfde81a497fa7a66590f9910aea
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357717B2

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