Triethylamine → HCID 66792810、化合物

HRID 534954

反応式

HRID 534954 の反応式
Cl.Cl.[C:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)([CH3:6])([CH3:5])[CH3:4].[NH:19]1[C@@H:23]([C:24](O)=[O:25])[CH2:22][CH2:21][C:20]1=[O:27].C(N(CC)CC)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>C(#N)C>[C:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N:13]1[CH2:18][CH2:17][N:16]([C:24]([C@@H:23]2[NH:19][C:20](=[O:27])[CH2:21][CH2:22]2)=[O:25])[CH2:15][CH2:14]1)([CH3:6])([CH3:4])[CH3:5]

参加物

7

反応物 5

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 439685D-Pyroglutamic acidHCID 667511491-(2-Tert-butylphenyl)piperazine dihydrochloride

生成物 1

HCID 66792810HCID 66792810、化合物収率 94%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1-(2-tert-butylphenyl)piperazine dihydrochloride obtained in Reference Example 1 (0.30 g, 1.03 mmol), (R)-(+)-2-pyrrolidone-5-carboxylic acid (0.15 g, 1.13 mmol), triethylamine (0.23 g, 2.26 mmol), EDCI (0.22 g, 1.13 mmol) and HOBt (0.17 g, 1.13 mmol) in acetonitrile (10 mL) was stirred at room temperature for 16 h. The reaction mixture was concentrated under reduced pressure and the resulting residue was partitioned between ethyl acetate and 10% sodium hydrogen carbonate solution. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting light pink solid was triturated with hexane to afford the title compound (0.32 g, 94%) as a light pink solid.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe resulting residue was partitioned between ethyl acetate and 10% sodium hydrogen carbonate solution
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting light pink solid was triturated with hexane

出典と根拠

ORDレコード
ord-d543783a08754cd2b6be7c79c7753305
出典データセット
uspto-grants-2014_10
特許番号
US08853215B2

関連ノート

読み込み中…