Triethylamine → HCID 178512830、化合物

HRID 65865ノート

反応式

HRID 65865 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH:5]([CH2:16][SH:17])[C:6]([N:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11])=[O:7].[N+]([O-])(O)=O.[C:22](C1C(C)=NNC=1C)(=[NH:24])[NH2:23].C(N(CC)CC)C>CN(C)C=O>[NH:1]([CH2:2][CH2:3][CH2:4][CH:5]([CH2:16][SH:17])[C:6]([N:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11])=[O:7])[C:22]([NH2:24])=[NH:23]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 127697271-(5-Amino-2-mercaptomethylpentanoyl)-L-prolineHCID 136347471Guanyl-3,5-dimethylpyrazole nitrate

生成物 1

HCID 178512830HCID 178512830、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 1-(5-amino-2-mercaptomethylpentanoyl)-L-proline (2.3 g), guanyl-3,5-dimethylpyrazole nitrate (2.41 g) and triethylamine (3.36 ml) in dimethylformamide (20 ml) is stored at room temperature under a blanket of argon for 16 hours. The solvents are removed in vacuo, the residue is dissolved in 0.1 N hydrochloric acid (10 ml) and zinc dust (500 mg) is added. The suspension is stirred at room temperature for 2 hours. After filtering, the filtrate is applied to a column of Dowex 50 ion exchange resin in the hydrogen cycle. The column is washed with water until no more acid is eluted and 1-(5-guanidino-2-mercaptomethylpentanoyl)-L-proline is then eluted with a pyridine-acetate buffer at pH 6.5.

後処理

  1. customThe solvents are removed in vacuo
  2. dissolutionthe residue is dissolved in 0.1 N hydrochloric acid (10 ml)
  3. additionzinc dust (500 mg) is added
  4. filtrationAfter filtering
  5. washThe column is washed with water until no more acid
  6. washis eluted
  7. wash1-(5-guanidino-2-mercaptomethylpentanoyl)-L-proline is then eluted with a pyridine-acetate buffer at pH 6.5

出典と根拠

ORDレコード
ord-a188190932c4445aa9703092ac96e6f2
出典データセット
uspto-grants-1978_12
特許番号
US04129571

反応ノート

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