Hydrochloric Acid → HCID 86601798、化合物

HRID 1394287ノート

反応式

HRID 1394287 の反応式
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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 86601797HCID 86601797、化合物

生成物 1

HCID 86601798HCID 86601798、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f6540c719ca9431785d4db43714af806
出典データセット
uspto-grants-2008_03
特許番号
US07348354B2

反応ノート

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