4-(5-Chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester → Hydrochloric Acid

HRID 1361517

反応式

HRID 1361517 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([C:16]2[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=2[O:23][CH3:24])([O:14][CH3:15])[CH2:10][CH2:9]1)=O)(C)(C)C>CO.Cl>[Cl:22][C:20]1[CH:19]=[CH:18][C:17]([O:23][CH3:24])=[C:16]([C:11]2([O:14][CH3:15])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:21]=1.[ClH:22]

参加物

4

反応物 1

HCID 587725284-(5-Chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester

生成物 2

HCID 313Hydrochloric AcidHCID 58772297HCID 58772297、化合物

試薬・触媒・溶媒 1

HCID 21893726Hydrochloride methanol溶媒

実験手順

A solution of 4-(5-chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester 5c (3.8 g, crude from last step) in methanol/HCl (2 M, 50 mL) was stirred at room temperature for 4 h, then the mixture was concentrated to half of volume under 40° C. and then ether was added. The precipitated was filtered and washed with ether to obtain 4-(5-chloro-2-methoxyphenyl)-4-methoxypiperidine 5d as its HCl salt. 1H NMR (DMSO-d6): δ 8.95 (b, 2H), 7.37-7.34 (q, J1=8.8 Hz, J2=8.8 Hz, 1H), 7.21-7.20 (d, J=2.8 Hz, 1H), 7.09-7.07 (d, J=8.8 Hz, 1H), 3.78 (s, 3H), 3.16-3.13 (m, 2H), 3.13-2.98 (m, 5H), 2.35-2.28 (m, 2H), 2.19-2.16 (m, 2H). ESI-MS m/z 256.8.

後処理

  1. concentrationthe mixture was concentrated to half of volume under 40° C.
  2. additionether was added
  3. filtrationThe precipitated was filtered
  4. washwashed with ether

出典と根拠

ORDレコード
ord-38d2ce59f83649bfb3dad518bd2060c6
出典データセット
uspto-grants-2011_02
特許番号
US07880007B2

関連ノート

読み込み中…