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Chlorotrimethylsilane → 2-[4-Dimethylamino-4-(3-fluorophenyl)cyclohexylidene]-N-[2-(1H-indol-3-yl)-1-methylethyl]acetamide hydrochloride

HRID 908957
ノート
印刷プレビュー

反応式

HRID 908957 の反応式
C[Si](C)(C)[Cl:3].[CH3:6][N:7]([CH3:37])[C:8]1([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([F:36])[CH:31]=2)[CH2:13][CH2:12][C:11](=[CH:14][C:15]([NH:17][CH:18]([CH3:29])[CH2:19][C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[NH:22][CH:21]=2)=[O:16])[CH2:10][CH2:9]1>CC(CC)=O>[ClH:3].[CH3:37][N:7]([CH3:6])[C:8]1([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([F:36])[CH:31]=2)[CH2:13][CH2:12][C:11](=[CH:14][C:15]([NH:17][CH:18]([CH3:29])[CH2:19][C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[NH:22][CH:21]=2)=[O:16])[CH2:10][CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6397ChlorotrimethylsilaneHCID 11712509HCID 11712509、化合物

生成物 1

HCID 117125082-[4-Dimethylamino-4-(3-fluorophenyl)cyclohexylidene]-N-[2-(1H-indol-3-yl)-1-methylethyl]acetamide hydrochloride

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

Trimethylchlorosilane (0.109 ml, 0.86 mmol) was added to a solution of the more polar diastereoisomer of 2-[4-dimethylamino-4-(3-fluorophenyl)cyclohexylidene]-N-[2-(1H-indol-3-yl)-1-methylethyl]acetamide (249 mg, 0.57 mmol) in ethyl methyl ketone (10 ml) and the mixture was stirred at RT for 1.5 h. The hydrochloride which had precipitated out was filtered off with suction and isolated as a colourless solid with an m.p. of 171-174° C. in a yield of 81% (218 mg) (Example 27).

後処理

  1. customThe hydrochloride which had precipitated out
  2. filtrationwas filtered off with suction
  3. customisolated as a colourless solid with an m.p. of 171-174° C. in a yield of 81% (218 mg) (Example 27)

出典と根拠

ORDレコード
ord-002604bdb4c347398a10abbb558496e6
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017630B2

反応ノート

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