Hydrochloric Acid → Hydrochloric Acid

HRID 711976노트

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HRID 711976 반응식
[OH:1][C@@H:2]([C:4]1[N:15]([C@H:16]2[CH2:21][CH2:20][C@H:19]([CH2:22][C:23]#[N:24])[CH2:18][CH2:17]2)[C:7]2=[C:8]3[S:14][CH:13]=[CH:12][C:9]3=[N:10][CH:11]=[C:6]2[N:5]=1)[CH3:3].[ClH:25].O>C(#N)C>[ClH:25].[OH:1][C@@H:2]([C:4]1[N:15]([C@H:16]2[CH2:21][CH2:20][C@H:19]([CH2:22][C:23]#[N:24])[CH2:18][CH2:17]2)[C:7]2=[C:8]3[S:14][CH:13]=[CH:12][C:9]3=[N:10][CH:11]=[C:6]2[N:5]=1)[CH3:3].[ClH:25]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 962Water2회HCID 178462237HCID 178462237, 화합물

생성물 2

HCID 313Hydrochloric AcidHCID 178462238HCID 178462238, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

(trans-4-{2-[(1R)-1-Hydroxyethyl]-1H-imidazo[4,5-d]thieno[3,2-b]pyridin-1-yl}cyclohexyl)acetonitrile (0.154 g, 0.451 mmol) was dissolved in acetonitrile (10 mL). 1.0 M Hydrogen chloride in water (0.480 mL, 0.480 mmol) was added slowly with stirring, followed by addition of water (10 mL). The mixture was stirred at room temperature until becoming homogeneous. The resulting solution was lyophilized to give the desired product as HCl salt. (0.169 g, 99.5%). LCMS calculated for C18H21N4OS (M+H)+: m/z=341.1. Found: 341.1. 1H NMR (DMSO-d6, 500 MHz) δ 9.55 (1H, s), 8.47 (1H, d, J=5.5 Hz), 8.00 (1H, d, J=5.5 Hz), 5.32 (1H, m), 5.07 (1H, m), 2.62 (2H, d, J=6.0 Hz), 2.43 (2H, m), 2.12 (2H, m), 2.04 (3H, m), 1.68 (3H, d, J=6.0 Hz), 1.46 (2H, m) ppm.

후처리

  1. stirringThe mixture was stirred at room temperature

출처 및 근거

ORD 기록
ord-bf7774a7147d47d6949546f133ec703a
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181271B2

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