tert-Butyl 4-carbamothioylpiperidine-1-carboxylate → 4-[4-(5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)thiazol-2-yl]piperidine

HRID 1401841ノート

反応式

HRID 1401841 の反応式
Br[CH2:2][C:3]([C:5]1[CH:14]=[CH:13][C:12]2[C:11]([CH3:16])([CH3:15])[CH2:10][CH2:9][C:8]([CH3:18])([CH3:17])[C:7]=2[CH:6]=1)=O.C(OC([N:26]1[CH2:31][CH2:30][CH:29]([C:32](=[S:34])[NH2:33])[CH2:28][CH2:27]1)=O)(C)(C)C>C(O)C>[CH3:15][C:11]1([CH3:16])[CH2:10][CH2:9][C:8]([CH3:18])([CH3:17])[C:7]2[CH:6]=[C:5]([C:3]3[N:33]=[C:32]([CH:29]4[CH2:30][CH2:31][NH:26][CH2:27][CH2:28]4)[S:34][CH:2]=3)[CH:14]=[CH:13][C:12]1=2

参加物

4

反応物 2

HCID 2735648tert-Butyl 4-carbamothioylpiperidine-1-carboxylateHCID 28013372-Bromo-1-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one

生成物 1

HCID 582464614-[4-(5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)thiazol-2-yl]piperidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

6.12 g (12.28 mmol) of 2-bromo-1-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethanone and 3 g (12.28 mmol) of 4-thiocarbamoylpiperidine-1-carboxylic acid tert-butyl ester were suspended in 50 ml of ethanol and refluxed overnight. The reaction mixture was cooled and evaporated. The residue was slurried using a little EA and PE, digested and filtered off with suction. The solid was suspended in 180 ml of EA, washed with 60 ml of a saturated sodium hydrogencarbonate solution. The organic phase was dried over sodium sulfate, filtered and evaporated.

後処理

  1. temperaturerefluxed overnight
  2. temperatureThe reaction mixture was cooled
  3. customevaporated
  4. filtrationfiltered off with suction
  5. washwashed with 60 ml of a saturated sodium hydrogencarbonate solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-91233daecc434ed0a6e7033d6d8cfde8
出典データセット
uspto-grants-2014_12
特許番号
US08907098B2

反応ノート

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