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Ammonia → Pivalic acid 6-{2-{[4-(2-amino-2-methylpropoxy)benzyl]ethylamino}-4-methoxyphenyl}-5,6,7,8-tetrahydronaphthalen-2-yl ester

HRID 1433996
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HRID 1433996 반응식
C(OC([NH:8][C:9]([CH3:48])([CH3:47])[CH2:10][O:11][C:12]1[CH:46]=[CH:45][C:15]([CH2:16][CH2:17][CH2:18][NH:19][C:20]2[CH:25]=[C:24]([O:26][CH3:27])[CH:23]=[CH:22][C:21]=2[CH:28]2[CH2:37][CH2:36][C:35]3[CH:34]=[C:33]([O:38][C:39](=[O:44])[C:40]([CH3:43])([CH3:42])[CH3:41])[CH:32]=[CH:31][C:30]=3[CH2:29]2)=[CH:14][CH:13]=1)=O)(C)(C)C.FC(F)(F)C(O)=O.O1CCCC1.N>ClCCl>[NH2:8][C:9]([CH3:48])([CH3:47])[CH2:10][O:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:16][CH2:17][CH2:18][NH:19][C:20]2[CH:25]=[C:24]([O:26][CH3:27])[CH:23]=[CH:22][C:21]=2[CH:28]2[CH2:37][CH2:36][C:35]3[CH:34]=[C:33]([O:38][C:39](=[O:44])[C:40]([CH3:41])([CH3:42])[CH3:43])[CH:32]=[CH:31][C:30]=3[CH2:29]2)=[CH:45][CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 6422Trifluoroacetic acidHCID 8028TetrahydrofuranHCID 66627582Pivalic acid 6-{2-{[4-(2-tert-butoxycarbonylamino-2-methylpropoxy)benzyl]ethylamino}-4-methoxyphenyl}-5,6,7,8-tetrahydronaphthalen-2-yl ester

생성물 1

HCID 66627097Pivalic acid 6-{2-{[4-(2-amino-2-methylpropoxy)benzyl]ethylamino}-4-methoxyphenyl}-5,6,7,8-tetrahydronaphthalen-2-yl ester
수율 94.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of pivalic acid 6-{2-{[4-(2-tert-butoxycarbonylamino-2-methylpropoxy)benzyl]ethylamino}-4-methoxyphenyl}-5,6,7,8-tetrahydronaphthalen-2-yl ester (90 mg) in dichloromethane (1.5 ml) was added trifluoroacetic acid (0.2 ml), and the solution was stirred for 1.5 hours at room temperature. The solution was neutralized by sequentially adding tetrahydrofuran and aqueous ammonia, extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (72 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. washsequentially washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated in vacuo
  5. customThe residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system)

출처 및 근거

ORD 기록
ord-5f79b2c5f5e3447ba839f72c42d53d33
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612114B2

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