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Dichloromethane → HCID 21077916, 화합물

HRID 1375073
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HRID 1375073 반응식
C([O:5][C:6](=[O:43])[CH2:7][C:8]1([C:13]2[CH:18]=[CH:17][C:16]([N:19]([C:21](=[O:42])[CH2:22][C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30]([NH:32][C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[CH3:39])=[O:31])=[C:25]([O:40][CH3:41])[CH:24]=3)[CH3:20])=[CH:15][CH:14]=2)[CH2:12][CH2:11][CH2:10][CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O.ClCCl>O>[CH3:41][O:40][C:25]1[CH:24]=[C:23]([CH2:22][C:21]([N:19]([CH3:20])[C:16]2[CH:17]=[CH:18][C:13]([C:8]3([CH2:7][C:6]([OH:43])=[O:5])[CH2:12][CH2:11][CH2:10][CH2:9]3)=[CH:14][CH:15]=2)=[O:42])[CH:28]=[CH:27][C:26]=1[NH:29][C:30]([NH:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=1[CH3:39])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 69420098[1-{4-[{2-[3-Methoxy-4-[3-o-tolyl-ureido]-phenyl]-acetyl}-methyl-amino]-phenyl}-cyclopentyl]-acetic acid tert-butyl ester

생성물 1

HCID 21077916HCID 21077916, 화합물수율 79.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

[1-{4-[{2-[3-Methoxy-4-[3-o-tolyl-ureido]-phenyl]-acetyl}-methyl-amino]-phenyl}-cyclopentyl]-acetic acid tert-butyl ester [0.18 g, Reference Example 8(b)] was treated with a mixture of trifluoroacetic acid (6 mL), dichloromethane (1.2 mL) and water (0.75 mL)and the resulting solution was then stirred at room temperature, under argon, for 1.5 hours. The amber coloured reaction mixture was evaporated and the residue was chased twice with toluene (20 mL) to yield an amber gum. This gum was triturated with pentane and the solid obtained was washed with pentane and then dried at 60° C., under vacuum, to give the title compound (0.13 g) as a pale yellow solid, m.p. softens at 100° C. then slowly melts from 118–150° C.

후처리

  1. customreaction mixture
  2. customwas evaporated
  3. customto yield an amber gum
  4. customThis gum was triturated with pentane
  5. customthe solid obtained
  6. washwas washed with pentane
  7. customdried at 60° C., under vacuum

출처 및 근거

ORD 기록
ord-b4fd66bc22854bfa9c53814ede105903
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166616B2

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