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4-Pentylaniline → HCID 67396887, 화합물

HRID 914514
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HRID 914514 반응식
[C:1]([CH2:4][C:5]1[N:6]=[C:7]([S:10][C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=[O:13])[S:8][CH:9]=1)(O)=O.[CH2:17]([C:22]1[CH:28]=[CH:27][C:25]([NH2:26])=[CH:24][CH:23]=1)[CH2:18][CH2:19][CH2:20][CH3:21]>O1CCCC1>[CH3:15][C:11]([S:10][C:7]1[S:8][CH:9]=[C:5]([CH2:4][CH2:1][NH:26][C:25]2[CH:27]=[CH:28][C:22]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:23][CH:24]=2)[N:6]=1)([CH3:16])[C:12]([OH:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 931624-PentylanilineHCID 67399201HCID 67399201, 화합물

생성물 1

HCID 67396887HCID 67396887, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

An operation similar to that of Example 520-1 was performed using 2-{[4-(carboxymethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid resin synthesized in Example 461-4 and 4-amylaniline (0.098 g) as starting materials. To the obtained resin were added tetrahydrofuran (2.0 mL) and 1 mol/L borane-tetrahydrofuran complex (2.0 mL), and the mixture was stirred at room temperature overnight. The resin was collected by filtration from the reaction mixture, washed once with tetrahydrofuran, twice with tetrahydrofuran/methanol=1:1 solution, and twice with methanol. Then, a solution (4.0 mL) of tetrahydrofuran-methanol-piperidine (1:1:2) was added to the resin, and the mixture was stirred at room temperature overnight. After completion of the reaction, the resin was collected by filtration, washed four times with tetrahydrofuran and twice with methanol, and vacuum dried to give the title pale-yellow resin (0.30 g).

후처리

  1. filtrationThe resin was collected by filtration from the reaction mixture
  2. washwashed once with tetrahydrofuran, twice with tetrahydrofuran/methanol=1:1 solution
  3. additionThen, a solution (4.0 mL) of tetrahydrofuran-methanol-piperidine (1:1:2) was added to the resin
  4. stirringthe mixture was stirred at room temperature overnight
  5. customAfter completion of the reaction
  6. filtrationthe resin was collected by filtration
  7. washwashed four times with tetrahydrofuran
  8. dry with materialtwice with methanol, and vacuum dried

출처 및 근거

ORD 기록
ord-0d9b47ecf33d4e9a96e7fafa3c408767
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08026370B2

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