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Trifluoroacetic acid → Trifluoroacetic acid

HRID 2370656
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반응식

HRID 2370656 반응식
C(OC([N:8]1[CH2:17][CH2:16][C:15]2[N:14]=[CH:13][C:12]([NH:18][C:19]3[N:28]=[C:27]4[C:22]([C:23](=[O:40])[N:24]([C:32]5[C:37]([F:38])=[CH:36][CH:35]=[CH:34][C:33]=5[Cl:39])[C:25]5[N:26]4[CH:29]=[CH:30][N:31]=5)=[CH:21][N:20]=3)=[CH:11][C:10]=2[CH2:9]1)=O)(C)(C)C.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]>C(Cl)Cl>[Cl:39][C:33]1[CH:34]=[CH:35][CH:36]=[C:37]([F:38])[C:32]=1[N:24]1[C:23](=[O:40])[C:22]2[CH:21]=[N:20][C:19]([NH:18][C:12]3[CH:13]=[N:14][C:15]4[CH2:16][CH2:17][NH:8][CH2:9][C:10]=4[CH:11]=3)=[N:28][C:27]=2[N:26]2[CH:29]=[CH:30][N:31]=[C:25]12.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 68193665HCID 68193665, 화합물

생성물 2

HCID 6422Trifluoroacetic acidHCID 68194960HCID 68194960, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of Example 277A (54.6 mg, 0.097 mmol) and trifluoroacetic acid (0.075 mL, 0.970 mmol) in CH2Cl2 (3 mL) was stirred overnight. The solids were filtered, rinsed with CH2Cl2, and dried to provide the title compound as a trifluoroacetic acid salt. 1H NMR (400 MHz, CD3OD) δ 3.29-3.26 (m, 2H), 3.68 (t, J=6.4 Hz, 2H), 4.55 (s, 2H), 7.11 (d, J=1.9 Hz, 1H), 7.44-7.35 (m, 1H), 7.56-7.53 (m, 1H), 7.66-7.60 (m, 1H), 7.91 (d, J=1.9 Hz, 1H), 8.38 (bs, 1H), 8.93 (bs, 1H), 9.26 (s, 1H). MS (ESI+) m/z 463.2 (M+H)+.

후처리

  1. filtrationThe solids were filtered
  2. washrinsed with CH2Cl2
  3. customdried

출처 및 근거

ORD 기록
ord-d009c0a95106491b92a6c846901d0951
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08710065B2

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