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

HRID 2264169노트

반응식

HRID 2264169 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 60209725HCID 60209725, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3d33b541611243158d50bb77c7698d2e
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855201B2

반응 노트

불러오는 중…