(2S,5S)-1-(4-tert-butylphenyl)-2,5-bis(4-nitrophenyl)pyrrolidine → A-1242846

HRID 1470937ノート

反応式

HRID 1470937 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C@H:15]([C:16]3[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][CH:17]=3)[CH2:14][CH2:13][C@H:12]2[C:25]2[CH:30]=[CH:29][C:28]([N+:31]([O-])=O)=[CH:27][CH:26]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]>CCCCCCC>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C@H:15]([C:16]3[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][CH:17]=3)[CH2:14][CH2:13][C@H:12]2[C:25]2[CH:30]=[CH:29][C:28]([NH2:31])=[CH:27][CH:26]=2)=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

3

反応物 1

HCID 86649103(2S,5S)-1-(4-tert-butylphenyl)-2,5-bis(4-nitrophenyl)pyrrolidine

生成物 1

HCID 67239053A-1242846

試薬・触媒・溶媒 1

HCID 8900Heptane溶媒

実験手順

To a 160 ml Parr stirrer hydrogenation vessel was added the product from Example 37D (2 g, 4.49 mmol), followed by 60 ml of THF, and Raney Nickel Grace 2800 (1 g, 50 wt % (dry basis)) under a stream of nitrogen. The reactor was assembled and purged with nitrogen (8×20 psig) followed by purging with hydrogen (8×30 psig). The reactor was then pressurized to 30 psig with hydrogen and agitation (700 rpm) began and continued for a total of 16 h at room temperature. The slurry was filtered by vacuum filtration using a GF/F Whatman glass fiber filter. Evaporation of the filtrate to afford a slurry followed by the addition heptane and filtration gave the crude title compound, which was dried and used directly in the next step.

後処理

  1. dry with materialfollowed by 60 ml of THF, and Raney Nickel Grace 2800 (1 g, 50 wt % (dry basis)) under a stream of nitrogen
  2. custompurged with nitrogen (8×20 psig)
  3. customby purging with hydrogen (8×30 psig)
  4. customcontinued for a total of 16 h at room temperature
  5. filtrationThe slurry was filtered by vacuum filtration
  6. filtrationfilter
  7. customEvaporation of the filtrate
  8. customto afford a slurry

出典と根拠

ORDレコード
ord-12f33ba0558a45d399e890783ed56d65
出典データセット
uspto-grants-2015_04
特許番号
US09006387B2

反応ノート

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