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Hydrochloric Acid → Isoindolin-5-yl(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)methanone

HRID 1808380
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HRID 1808380 반응식
Cl.[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[CH:20]=[C:21]5[C:25](=[CH:26][CH:27]=4)[CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22]5)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[CH2:24]1[C:25]2[C:21](=[CH:20][C:19]([C:17]([N:14]3[CH2:13][CH2:12][C:11]4([CH2:35][CH2:36][N:8]([C:5]5[CH:6]=[CH:7][N:2]=[CH:3][CH:4]=5)[CH2:9][CH2:10]4)[CH2:16][CH2:15]3)=[O:18])=[CH:27][CH:26]=2)[CH2:22][NH:23]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59483841tert-Butyl 5-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)isoindoline-2-carboxylate

생성물 1

HCID 59483811Isoindolin-5-yl(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)methanone

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

1.25 M hydrogen chloride in methanol (7.1 ml, 8.92 mmol) was added at RT to a solution of tert-butyl 5-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)isoindoline-2-carboxylate (0.85 g, 1.78 mmol) in methanol (1 ml), and the reaction mixture was refluxed for 1 h. The solvent was removed in vacuo, the residue was taken up in a small amount of ethanol (2 ml), and diethyl ether (50 ml) was added. The mixture was then cooled for 30 min in an ice bath, and the resulting solid was filtered out, washed with diethyl ether and dried in vacuo. Yield: 0.74 g (92%).

후처리

  1. temperaturethe reaction mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureThe mixture was then cooled for 30 min in an ice bath
  5. filtrationthe resulting solid was filtered out
  6. washwashed with diethyl ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-ce308bd8500444c68b5fc3a12e04cec2
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08357717B2

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