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Hydrochloric Acid → HCID 178483517, 화합물

HRID 424546
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HRID 424546 반응식
[CH3:1][N:2]([CH3:24])[CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][S:9][C:8]2[CH:12]=[C:13]([NH:16][C:17]([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)=[NH:18])[CH:14]=[CH:15][C:7]1=2.[ClH:25]>CO>[ClH:25].[ClH:25].[CH3:24][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][S:9][C:8]2[CH:12]=[C:13]([NH:16][C:17]([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)=[NH:18])[CH:14]=[CH:15][C:7]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178483516HCID 178483516, 화합물

생성물 1

HCID 178483517HCID 178483517, 화합물수율 99%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of N-(4-(3-(dimethylamino)propyl)-3,4-dihydro-2H-benzo[b][1,4]thiazin-7-yl)thiophene-2-carboximidamide (0.16 g, 0.444 mmol) in dry methanol (5 mL) was treated with hydrogen chloride (1M solution in ether; 1.331 mL, 1.331 mmol) at room temperature. The mixture was stirred for 15 minutes, the solvent was evaporated, and the residue was dried under high vacuum to obtain the title product (0.19 g, 99%) as a solid. 1H NMR (DMSO-d6) δ 11.22 (s, 1H), 10.91 (brs, 1H), 9.67 (s, 1H), 8.69 (s, 1H), 8.15-8.11 (m, 2H), 7.36 (t, 1H, J=4.5 Hz), 7.04-6.88 (m, 3H), 3.64-3.61 (m, 2H), 3.41 (t, 2H, J=6.9 Hz), 3.14-3.02 (m, 4H), 2.72 (d, 6H, J=4.8 Hz), 2.06-1.98 (m, 2H); ESI-MS (m/z, %): 361 (MH+, free base, 91), 276 (100); ESI-HRMS calculated for C18H25N4S2 (MH+, free base), calculated: 361.1515, observed: 361.1515; HPLC purity: 98.15% by area.

후처리

  1. customthe solvent was evaporated
  2. customthe residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-21295280421b4a39ad1c3085cbbbd625
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106043B2

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