Hydrochloric Acid → HCID 69083351, 화합물

HRID 1525848노트

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HRID 1525848 반응식
[CH:1]1([N:4]2[CH2:9][C:8]3([CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]3)[O:7][CH2:6][C:5]2=[O:22])[CH2:3][CH2:2]1.[ClH:23]>C(O)C.O1CCOCC1>[ClH:23].[CH:1]1([N:4]2[CH2:9][C:8]3([CH2:10][CH2:11][NH:12][CH2:13][CH2:14]3)[O:7][CH2:6][C:5]2=[O:22])[CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 690854321,1-Dimethylethyl 4-cyclopropyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate

생성물 1

HCID 69083351HCID 69083351, 화합물수율 58%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

1,1-Dimethylethyl 4-cyclopropyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate was dissolved in ethanol (300 mL) and cooled over an ice bath. A 4M solution of hydrogen chloride in dioxane (300 mL) was added, such that the temperature remained low. The ice bath was removed and the mixture was stirred at ambient temperature overnight. The solid was collected, washed with a little ethanol and diethyl ether to give the title product (47.1 g, 58%). The mother liquors were treated with diethyl ether (1.2 L), stirred for 30 min, and the solid was collected and dried to give a total combined yield of 78% of the title product (63.69 g) over the three steps. MS(ES)+ m/e 211.0[M+H+]; 1H NMR (400 MHz, DMSO-d6) δ 9.17-8.64 (m, 2 H), 4.04 (s, 2 H), 3.14 (d, J=13.1 Hz, 2 H), 3.01-2.85 (m, 2 H), 2.83-2.71 (m, 1 H), 1.96-1.83 (m, 2 H), 1.83-1.68 (m, 2 H), 0.76-0.67 (m, 2 H), 0.64-0.55 (m, 2 H).

후처리

  1. temperaturecooled over an ice bath
  2. customThe ice bath was removed
  3. customThe solid was collected
  4. washwashed with a little ethanol and diethyl ether

출처 및 근거

ORD 기록
ord-861792737eba48ada612069cc5f96277
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09084794B2

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