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Potassium Carbonate → tert-Butyl (S)-5-amino-3,4-dihydro-2H-pyrrole-2-carboxylate

HRID 481238
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반응식

HRID 481238 반응식
Cl.[NH2:2][C:3]1[CH2:4][CH2:5][C@@H:6]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[N:7]=1.C([O-])([O-])=O.[K+].[K+]>C(Cl)(Cl)Cl>[NH2:2][C:3]1[CH2:4][CH2:5][C@@H:6]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 70094840tert-Butyl (S)-5-amino-3,4-dihydro-2H-pyrrole-2-carboxylate hydrochloride

생성물 1

HCID 53795147tert-Butyl (S)-5-amino-3,4-dihydro-2H-pyrrole-2-carboxylate수율 93%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Amidine hydrochloride 1d (11.0 g, 49.8 mmol) was partitioned between CHCl3 and sat. K2CO3. The layers were separated and the aqueous layer was extracted with CHCl3 (2×). The combined organic phase was dried (Na2SO4) and concentrated to afford 8.50 g (93%) of free base 1e. 1H NMR (300 MHz, CDCl3) δ4.44 (br s, 2H), 4.38 (dd, J=8.0, 5.5, 1H), 2.65-2.42 (m, 2H), 2.32-2.18 (m, 1H), 2.12-2.00 (m, 1H), 1.47 (s, 9H).

후처리

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with CHCl3 (2×)
  3. dry with materialThe combined organic phase was dried (Na2SO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1f3fc0f97d68417db59ed98fa2bac4c2
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06653295B2

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