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1,2-Dibromoethane → (1RS,2RS,4SR)-2-dimethylaminomethyl-4-isobutoxy-(3-methylsulphanyl-phenyl)-cyclohexanol hydrochloride

HRID 2392745
ノート
印刷プレビュー

反応式

HRID 2392745 の反応式
Cl.[CH3:2][N:3]([CH2:5][CH:6]1[CH2:11][CH:10]([O:12][CH2:13][CH:14]([CH3:16])[CH3:15])[CH2:9][CH2:8][C:7]1=[O:17])[CH3:4].Br[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([S:25][CH3:26])[CH:20]=1.BrCCBr.C[Si](C)(C)[Cl:33].O>CCOCC>[ClH:33].[CH3:4][N:3]([CH2:5][CH:6]1[CH2:11][CH:10]([O:12][CH2:13][CH:14]([CH3:15])[CH3:16])[CH2:9][CH2:8][C:7]1([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([S:25][CH3:26])[CH:20]=1)[OH:17])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 78391,2-DibromoethaneHCID 27356273-BromothioanisoleHCID 189805002-Dimethylaminomethyl-4-isobutoxy-cyclohexanone hydrochlorideHCID 86753056Chlorotrimethylsilane water

生成物 1

HCID 18980483(1RS,2RS,4SR)-2-dimethylaminomethyl-4-isobutoxy-(3-methylsulphanyl-phenyl)-cyclohexanol hydrochloride収率 32%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Compound (22) was reacted with 1-bromo-3-methylsulphanyl-benzene corresponding to the conditions described in Example 1. In departure from the conditions described in Example 1, ether was used as the solvent and 1,2-dibromoethane was added to the batch in order to increase the yield. The crude product obtained was purified with diisopropyl ether via a silica gel column, and was taken up in tetrahydrofuran/ether. The crystals obtained after adding trimethylchlorosilane/water were recrystallised from ethyl acetate. Compound (23) was obtained in a yield of 32% theoretical.

後処理

  1. additionwas added to the batch in order
  2. temperatureto increase the yield
  3. customThe crude product obtained
  4. customwas purified with diisopropyl ether via a silica gel column
  5. customThe crystals obtained
  6. customwere recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-677f11368ebe4dfa8730a75190011983
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05801201

反応ノート

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