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Hydrochloric Acid → HCID 18700185, 화합물

HRID 2289340
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HRID 2289340 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH2:21][C:22]([N:24]3[CH2:29][CH2:28][CH:27]([N:30]4[C:39]5[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=5)[CH2:33][CH2:32][C:31]4=[O:40])[CH2:26][CH2:25]3)=[O:23])=[C:17]([O:41][CH2:42][C:43]([F:46])([F:45])[F:44])[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CCOC(C)=O>[NH:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH2:21][C:22]([N:24]3[CH2:25][CH2:26][CH:27]([N:30]4[C:39]5[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=5)[CH2:33][CH2:32][C:31]4=[O:40])[CH2:28][CH2:29]3)=[O:23])=[C:17]([O:41][CH2:42][C:43]([F:44])([F:45])[F:46])[CH:16]=2)[CH2:10][CH2:9]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 18700143HCID 18700143, 화합물

생성물 1

HCID 18700185HCID 18700185, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

Into a stirred solution of (N-tert-butyloxycarbonyl-4-piperidinyloxy)-2-(2,2,2-trifluoroethoxy)phenylacetyl)-piperidin-4-yl)-3,4-dihydroquinolin-2(1H)-one (1.2 g, 1.8 mmol) from Step 1 above in EtOAc (75 mL) at 0° C. was bubbled HCl gas for 15 min. The resulting suspension was stirred at 0° C. for 45 min. Excess HCl was removed by bubbling argon though the mixture for 15 min. Ether (150 mL) was added and the cold suspension was filtered. The solids were washed with additional ether and then dried under reduced pressure for 18 h to give the hydrochloride salt of the title compound as an amorphous white powder.

후처리

  1. customExcess HCl was removed
  2. customby bubbling argon though the mixture for 15 min
  3. additionEther (150 mL) was added
  4. filtrationthe cold suspension was filtered
  5. washThe solids were washed with additional ether
  6. customdried under reduced pressure for 18 h

출처 및 근거

ORD 기록
ord-3469fd3181b843acb0b80a4922765f53
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090805

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