HCID 13599173、化合物 → N-(3-mercapto-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester

HRID 543262ノート

反応式

HRID 543262 の反応式
[C:1]([O:5][C:6](=[O:23])[CH2:7][N:8]([C:14](=[O:22])[CH:15]([CH3:21])[CH2:16][S:17]C(=O)C)[CH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1)([CH3:4])([CH3:3])[CH3:2]>CO>[C:1]([O:5][C:6](=[O:23])[CH2:7][N:8]([C:14](=[O:22])[CH:15]([CH3:21])[CH2:16][SH:17])[CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13]1)([CH3:3])([CH3:2])[CH3:4]

参加物

3

反応物 1

HCID 13599173HCID 13599173、化合物

生成物 1

HCID 13469597N-(3-mercapto-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester収率 71.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Into a solution containing 50 g (0.14 mol) of N-(3-acetylthio-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester in 700 ml of methanol was bubbled nitrogen gas for 10 minutes followed by ammonia gas for 30 minutes. After 30 minutes the mixture was concentrated in vacuo and the residue taken up in ethyl acetate. It was washed once with 3% aqueous HCl and once with water, dried over MgSO4, filtered, and concentrated in vacuo to yield an oily product. Purification via HPLC [15% ethyl acetate in hexanes] afforded 30 g (70%) of N-(3-mercapto-2-methyl-propanoyl)-N-cyclopentylglycine t-butyl ester as an oil.

後処理

  1. customwas bubbled nitrogen gas for 10 minutes
  2. concentrationAfter 30 minutes the mixture was concentrated in vacuo
  3. washIt was washed once with 3% aqueous HCl and once with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto yield an oily product
  8. customPurification via HPLC [15% ethyl acetate in hexanes]

出典と根拠

ORDレコード
ord-b14897b205bf4a40bedf678558b91e01
出典データセット
uspto-grants-1987_04
特許番号
US04661515

反応ノート

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