Trifluoroacetic acid → HCID 20729748, 화합물

HRID 352175노트

반응식

HRID 352175 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([CH2:15][NH:16][C:17]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:18])[CH2:10]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>>[CH2:20]([O:19][C:17](=[O:18])[NH:16][CH2:15][C@@H:11]1[CH2:12][CH2:13][CH2:14][C@H:9]([NH2:8])[CH2:10]1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 22713895[3-(Benzyloxycarbonylamino-methyl)-cyclohexyl]-carbamic acid tert-butyl ester

생성물 1

HCID 20729748HCID 20729748, 화합물

실험 절차

S-amino enantiomer of N-({3-[(t-butoxy)carbonyl-amino]cyclohexyl}methyl) (phenylmethoxy)carboxamide (1.0 g, 2.76 mmol) was treated with TFA (5 mL) under N2. After 20 min of stirring at r.t. the reaction was complete. The crude was then concentrated to an oil which was purified on a Varian Bond-Elut SCX column (10 g). The column was eluted consecutively with CHCl3, MeOH, and ammonia (2.0M in MeOH). The pure product was recovered from the ammonia fractions. The solvent was removed in vacuo to afford 0.632 g (87%) as a colorless oil. MS (ES+) m/z 263.0 (M+H)+.

후처리

  1. concentrationThe crude was then concentrated to an oil which
  2. customwas purified on a Varian Bond-Elut SCX column (10 g)
  3. washThe column was eluted consecutively with CHCl3, MeOH, and ammonia (2.0M in MeOH)
  4. customThe pure product was recovered from the ammonia fractions
  5. customThe solvent was removed in vacuo
  6. customto afford 0.632 g (87%) as a colorless oil

출처 및 근거

ORD 기록
ord-dd66de9effbc43ffa8f6b4d193a621bb
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743794B2

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