Hydrochloric Acid → HCID 86601798, 화합물

HRID 1394287노트

반응식

HRID 1394287 반응식
Cl.[CH3:2][N:3]([CH3:33])[C:4]1([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][NH:12][C:13]([NH:15][CH2:16][CH2:17][C:18]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[NH:20][CH:19]=2)=[S:14])[CH2:6][CH2:5]1.C[Si](C)(C)[Cl:36]>CC(CC)=O>[ClH:36].[CH3:33][N:3]([CH3:2])[C:4]1([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][NH:12][C:13]([NH:15][CH2:16][CH2:17][C:18]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[NH:20][CH:19]=2)=[S:14])[CH2:6][CH2:5]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 86601797HCID 86601797, 화합물

생성물 1

HCID 86601798HCID 86601798, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

In order to produce the hydrochloride, the more nonpolar diastereoisomer of 1-[2-(4-dimethylamino-4-phenylcyclohexyl)ethyl]-3-[2-(1H-indol-3-yl)ethyl]thiourea (230 mg, 0.5 mmole) was dissolved in ethyl methyl ketone (5 ml) and combined with trimethylchlorosilane (2.5 ml, 26.8 mmole). The colorless solid which precipitated out was removed by suction filtration after 2 h, washed with ethyl methyl ketone (3×5 ml) and then dried. The more nonpolar diastereoisomer of 1-[2-(4-dimethylamino-4-phenylcyclohexyl)-ethyl]-3-[2-(1H-indol-3-yl)ethyl]thiourea hydrochloride was obtained in this manner as a colorless solid (Example 43, m.p. 130-138° C.) in a yield of 240 mg (99%).

후처리

  1. customThe colorless solid which precipitated out
  2. customwas removed by suction filtration after 2 h
  3. washwashed with ethyl methyl ketone (3×5 ml)
  4. customdried

출처 및 근거

ORD 기록
ord-f6540c719ca9431785d4db43714af806
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07348354B2

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