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Hydrochloric Acid → neopentyl ((S)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)methylcarbamate hydrochloride

HRID 2062354
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HRID 2062354 반응식
[CH2:1]([O:6][C:7](=[O:33])[NH:8][CH2:9][C@@H:10]1[CH2:14][CH2:13][N:12]([C:15]2[C:24]3[C:19](=[CH:20][C:21]([CH3:25])=[CH:22][CH:23]=3)[N:18]=[C:17]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[OH:32])[N:16]=2)[CH2:11]1)[C:2]([CH3:5])([CH3:4])[CH3:3].[ClH:34].CCOCC>C(Cl)Cl>[ClH:34].[OH:32][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=1[C:17]1[N:16]=[C:15]([N:12]2[CH2:13][CH2:14][C@@H:10]([CH2:9][NH:8][C:7](=[O:33])[O:6][CH2:1][C:2]([CH3:3])([CH3:4])[CH3:5])[CH2:11]2)[C:24]2[C:19](=[CH:20][C:21]([CH3:25])=[CH:22][CH:23]=2)[N:18]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl Ether2회HCID 136121466neopentyl((S)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)methylcarbamate

생성물 1

HCID 136330122neopentyl ((S)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)methylcarbamate hydrochloride수율 92%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

A solution of neopentyl((S)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)methylcarbamate (215 mg, 0.48 mmol) in CH2Cl2 (2 ml) was stirred under an N2 atmosphere. A 1.0 M HCl solution in ether (0.48 ml, 0.48 mmol) was added dropwise to this solution. After 10 minutes, ether (8 ml) was added until a precipitate formed, which was filtered and dried to obtain neopentyl ((S)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)methylcarbamate hydrochloride (214 mg, 92%). LC/MS: m/z 449 (M+H)+ at 2.75 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

후처리

  1. customformed
  2. filtrationwhich was filtered
  3. customdried

출처 및 근거

ORD 기록
ord-f72da48263db418487646d10b17befb5
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283354B2

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