Hydrochloric Acid → (+/-)-N-isobutyl-N-(2,3,4,5-tetrahydro-1-benzoxepin-8-ylmethyl)morpholine-2-carboxamide hydrochloride

HRID 2264169ノート

反応式

HRID 2264169 の反応式
[CH2:1]([N:5]([CH2:21][C:22]1[CH:32]=[CH:31][C:25]2[CH2:26][CH2:27][CH2:28][CH2:29][O:30][C:24]=2[CH:23]=1)[C:6]([CH:8]1[O:13][CH2:12][CH2:11][N:10](C(OC(C)(C)C)=O)[CH2:9]1)=[O:7])[CH:2]([CH3:4])[CH3:3].[ClH:33]>O1CCOCC1>[ClH:33].[CH2:1]([N:5]([CH2:21][C:22]1[CH:32]=[CH:31][C:25]2[CH2:26][CH2:27][CH2:28][CH2:29][O:30][C:24]=2[CH:23]=1)[C:6]([CH:8]1[O:13][CH2:12][CH2:11][NH:10][CH2:9]1)=[O:7])[CH:2]([CH3:4])[CH3:3]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 60209725HCID 60209725、化合物

生成物 1

HCID 60209726(+/-)-N-isobutyl-N-(2,3,4,5-tetrahydro-1-benzoxepin-8-ylmethyl)morpholine-2-carboxamide hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 0.798 g (1.79 mmol) of (±)-tert-butyl 2-{[isobutyl(2,3,4,5-tetrahydro-1-benzoxepin-8-ylmethyl)amino]carbonyl}morpholine-4-carboxylate in 3.6 mL of dioxane cooled in an ice-bath was added 3.6 mL (14.4 mmol, 8 equiv) of 4M HCl in dioxane. The solution was stirred 30 minutes with cooling, then for 3.5 hours at ambient temperature. The solution was concentrated under reduced pressure, the residue triturated with ether, and dried under vacuum to give the product as a white solid. MS (m+1)=347.3; H NMR (400 MHz, CD3OD) 7.12 (m, 1H), 6.84 (m, 2H), 4.8-4.6 (m, 2H), 4.58-4.39 (m, 1H), 4.1-3.85 (m, 4H), 3.5-3.35 (m, 3H), 3.24 (m, 2H), 3.15-2.92 (m, 1H), 2.78 (m, 2H), 2.02 (m, 1H), 1.95 (m, 2H), 1.71 (m, 2H), 0.89 (m, 6H).

後処理

  1. temperaturewith cooling
  2. waitfor 3.5 hours at ambient temperature
  3. concentrationThe solution was concentrated under reduced pressure
  4. customthe residue triturated with ether
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-3d33b541611243158d50bb77c7698d2e
出典データセット
uspto-grants-2010_12
特許番号
US07855201B2

反応ノート

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