Hydrochloric Acid → {4-[4-(2-Aminoethoxy)phenyl]butyl}carbamic acid benzyl ester hydrochloride

HRID 217933노트

반응식

HRID 217933 반응식
[CH2:1]([O:8][C:9](=[O:32])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][NH:24]C(OC(C)(C)C)=O)=[CH:17][CH:16]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:33].CCOCC>CO.C1COCC1>[ClH:33].[CH2:1]([O:8][C:9](=[O:32])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][NH2:24])=[CH:17][CH:16]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 67364654{4-[4-(2-tert-Butoxycarbonylaminoethoxy)phenyl]butyl}carbamic acid benzyl ester

생성물 1

HCID 66849606{4-[4-(2-Aminoethoxy)phenyl]butyl}carbamic acid benzyl ester hydrochloride

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

{4-[4-(2-tert-Butoxycarbonylaminoethoxy)phenyl]butyl}carbamic acid benzyl ester 1 (11.0 g, 24.9 mmol) was dissolved in methanol (110 mL) and THF (20 mL). 12N Hydrochloric acid (40 mL) was added dropwise, and the reaction was allowed to stir. After 1.5 h, ether (200 mL) was added, and the reaction was suction filtered to collect a white solid. The solid was washed with ether, air dried, and dried under vacuum. This afforded 7.6 g, (82%) of 7 as a white solid. 1H NMR (300 MHz, CD3OD) δ 1.39 (br s, 11H), 1.52 (m, 2H).

후처리

  1. filtrationfiltered
  2. customto collect a white solid
  3. washThe solid was washed with ether, air
  4. customdried
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-7d1d4873825446b8b46cfc12a79799a7
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198286B2

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