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Trifluoroacetic acid → HCID 178504906, 화합물

HRID 1257725
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반응식

HRID 1257725 반응식
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([S:14]([CH3:17])(=[O:16])=[O:15])[CH2:10][CH2:9]1)(C)(C)C.[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22]>C(Cl)Cl>[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22].[CH3:17][S:14]([C@H:11]1[CH2:12][CH2:13][C@H:8]([NH2:7])[CH2:9][CH2:10]1)(=[O:15])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 178454083HCID 178454083, 화합물

생성물 1

HCID 178504906HCID 178504906, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A suspension of trans (4-methanesulfonyl-cyclohexyl)-carbamic acid tert-butyl ester (0.40 g, 1.40 mmol) in DCM (5 mL) was treated with trifluoroacetic acid (5 mL) and the mixture was stirred at ambient temperature for 30 minutes then concentrated under vacuum. The residue was azeotroped with toluene (×2) and the resulting oil was triturated (diethyl ether) to provide a solid which was washed with ether and dried to give 386 mg (93%) of trans 4-methanesulfonyl-cyclohexylamine trifluoroacetic acid salt as a white solid. 1H NMR (400 MHz, DMSO) δ: 7.86 (s, 3H), 3.11-2.98 (m, 2H), 2.92 (s, 3H), 2.18-2.02 (m, 4H), 1.56-1.43 (m, 2H), 1.43-1.28 (t, 2H).

후처리

  1. concentrationthen concentrated under vacuum
  2. customThe residue was azeotroped with toluene (×2)
  3. customthe resulting oil was triturated (diethyl ether)
  4. customto provide a solid which
  5. washwas washed with ether
  6. customdried

출처 및 근거

ORD 기록
ord-7d17196c44964e14bc31803dfaff1eec
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461328B2

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