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Hydrochloric Acid → HCID 86672469, 화합물

HRID 712969
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HRID 712969 반응식
[F:1][CH:2]([F:28])[CH2:3][N:4]1[CH2:21][CH:20]([C:22]2[NH:26][N:25]=[CH:24][C:23]=2[CH3:27])[O:19][C:6]2([CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8][CH2:7]2)[CH2:5]1.Cl.Cl.FC(F)CN1CC(C2NN=CC=2C)OC2(CCNCC2)C1>C(O)C>[F:28][CH:2]([F:1])[CH2:3][N:4]1[CH2:21][CH:20]([C:22]2[NH:26][N:25]=[CH:24][C:23]=2[CH3:27])[O:19][C:6]2([CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 86672470tert-butyl 8-(2,2-difluoroethyl)-10-(4-methyl-1H-pyrazol-5-yl)-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylateHCID 86672471HCID 86672471, 화합물

생성물 1

HCID 86672469HCID 86672469, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To tert-butyl 8-(2,2-difluoroethyl)-10-(4-methyl-1H-pyrazol-5-yl)-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylate (80 mg, 0.20 mmol) in ethanol (0.2 mL) was added HCl (500 μL of 4 M in dioxane, 2.00 mmol) and the reaction mixture was stirred for 1 hour. The reaction mixture was concentrated in vacuo to give, 8-(2,2-difluoroethyl)-10-(4-methyl-1H-pyrazol-5-yl)-11-oxa-3,8-diazaspiro[5.5]undecane hydrochloride salt as a yellow solid. ESI-MS m/z calc. 300.2. found 301.3 (M+1)+; Retention time: 0.48 minutes (3 min run). 1H NMR (400 MHz, DMSO) δ 8.74 (s, 2H), 7.45 (s, 1H), 6.49-6.08 (m, 1H), 5.76 (s, 1H), 4.88 (d, J=9.6 Hz, 1H), 3.21-2.57 (m, 10H), 2.06 (s, 3H), 1.81-1.56 (m, 4H).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customto give
  3. customRetention time: 0.48 minutes (3 min run)

출처 및 근거

ORD 기록
ord-d887a24b043e42e3bfae4ae8a14d5be0
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181273B2

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