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

HRID 81325ノート

反応式

HRID 81325 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

{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),

後処理

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

出典と根拠

ORDレコード
ord-bc0af1aee9554cd6a1fa3fff2feb53ed
出典データセット
uspto-grants-2014_09
特許番号
US08846688B2

反応ノート

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