HCID 13599173, 화합물 → N-(3-mercapto-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester

HRID 543262노트

반응식

HRID 543262 반응식
[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]

참가 물질

3

반응물 1

HCID 13599173HCID 13599173, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-b14897b205bf4a40bedf678558b91e01
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04661515

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