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Hydrochloric Acid → (4-Fluoro-3-trifluoromethyl-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-amine hydrochloride

HRID 589600
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HRID 589600 반응식
C(OC(=O)[N:7]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[C:21]([C:26]([F:29])([F:28])[F:27])[CH:20]=1)[C:8]1[S:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]=1[CH3:17])(C)(C)C.[ClH:31]>O1CCOCC1.CCOCC>[ClH:31].[F:25][C:22]1[CH:23]=[CH:24][C:19]([CH2:18][NH:7][C:8]2[S:12][C:11]3[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=3[C:9]=2[CH3:17])=[CH:20][C:21]=1[C:26]([F:29])([F:27])[F:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 59376673(4-Fluoro-3-trifluoromethyl-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 67426625(4-Fluoro-3-trifluoromethyl-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-amine hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

실험 절차

To compound 6-C was added a solution of 4N HCl in dioxane (20 mL) and the reaction mixture was stirred for 3 hours. The reaction mixture was diluted with ether, the solid filtered, washed with ether, and dried under vacuo to afford 1.86 g of compound 6-D as a white solid. 1H NMR (CD3OD, 300 MHz): δ 7.61-7.83 (m, 3H), 7.52 (d, 1H), 7.26-7.39 (m, 2H), 7.10-7.26 (m, 1H), 4.57 (s, 2H), 2.22 (s, 3H); MS (method 2): m/z 340.0 (MH+); HPLC (method 1): Rt 6.78 minutes.

후처리

  1. filtrationthe solid filtered
  2. washwashed with ether
  3. customdried under vacuo
  4. customto afford 1.86 g of compound 6-D as a white solid

출처 및 근거

ORD 기록
ord-d08f382244664e9eaa3e472e0d4289ee
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09233947B2

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