7-Methylene-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene → 7-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene

HRID 1013412

反応式

HRID 1013412 の反応式
[CH2:1]=[C:2]1[C:9]2[S:8][CH:7]=[CH:6][C:5]=2[CH:4]2[CH2:10][N:11]([CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH3:14])[CH2:12][CH:3]12>CO.[Pd]>[CH3:1][CH:2]1[C:9]2[S:8][CH:7]=[CH:6][C:5]=2[CH:4]2[CH2:10][N:11]([CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH3:14])[CH2:12][CH:3]12

参加物

4

反応物 1

HCID 1317290307-Methylene-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene

生成物 1

HCID 1317270457-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene収率 72.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
35 °C

実験手順

The product of step f) (226 mg, 0.80 mmol) was added to a suspension of 10% Pd/C (339 mg) in 8 mL of methanol. The reaction chamber was evacuated from air and was filled with H2 (1 atm). The reaction mixture was stirred under H2 for 12 hours at 35° C. The reaction mixture was filtered through Celite and evaporated in vacuo to give the subtitle compound as an oil (165 mg, 72.5%). MS calculated for C18H21NS +H: 284, observed: 284.

後処理

  1. customThe reaction chamber was evacuated from air
  2. additionwas filled with H2 (1 atm)
  3. filtrationThe reaction mixture was filtered through Celite
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9bd6b05a3dca4595be94c55efbf0c7a4
出典データセット
uspto-grants-2011_07
特許番号
US07981919B2

関連ノート

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