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Hydrochloric Acid → HCID 178445631, 화합물

HRID 1350611
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HRID 1350611 반응식
[CH2:1]([O:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[C:7]([F:15])[C:8]([F:14])=[CH:9][CH:10]=2)[C:5]=1[F:16])[CH3:2].C([Li])CCC.CCCCCC.[CH2:28]([C@H:32]1[CH2:37][CH2:36][C@H:35]([C@H:38]2[CH2:43][CH2:42][C@H:41]([CH2:44][CH:45]=[O:46])[CH2:40][CH2:39]2)[CH2:34][CH2:33]1)[CH2:29][CH2:30][CH3:31].Cl>O1CCCC1>[CH2:1]([O:3][C:4]1[C:5]([F:16])=[C:6]2[C:11]([CH:10]=[C:9]([CH:45]([OH:46])[CH2:44][C@H:41]3[CH2:40][CH2:39][C@H:38]([C@H:35]4[CH2:36][CH2:37][C@H:32]([CH2:28][CH2:29][CH2:30][CH3:31])[CH2:33][CH2:34]4)[CH2:43][CH2:42]3)[C:8]([F:14])=[C:7]2[F:15])=[CH:12][CH:13]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 23077311HCID 23077311, 화합물HCID 178418244HCID 178418244, 화합물HCID 178445633HCID 178445633, 화합물

생성물 1

HCID 178445631HCID 178445631, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

A tetrahydrofuran (50 ml) solution of 2-ethoxy-1,7,8-trifluoronaphthalene (9.4 g) was cooled to −60° C. Then, a 1.58 M butyllithium/hexane solution (47 ml) was added dropwise to this solution, followed by stirring for 2 hours. A tetrahydrofuran (50 ml) solution of trans-4-(trans-4-butylcyclohexyl)cyclohexylacetoaldehyde (13.2 g) was added dropwise at −50° C. . After stirring for 2 hours, the reaction temperature was increased to 0° C. 10% hydrochloric acid was added to the reaction solution. The reaction solution was extracted with ethyl acetate, washed with brine, and concentrated. The residue was recrystallized from ethyl acetate, and 7-ethoxy-3-[2-[trans-4-(trans-4-butylcyclohexyl)cyclohexyl]-1-hydroxyethyl]-1,2,8-trifluoronaphthalene was obtained.

후처리

  1. stirringAfter stirring for 2 hours
  2. extractionThe reaction solution was extracted with ethyl acetate
  3. washwashed with brine
  4. concentrationconcentrated
  5. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-26bcfdd441c74d77bb65c9e4d0703101
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214835B2

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