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4-Pentylaniline → HCID 67396887、化合物

HRID 914514
ノート
印刷プレビュー

反応式

HRID 914514 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 931624-PentylanilineHCID 67399201HCID 67399201、化合物

生成物 1

HCID 67396887HCID 67396887、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0d9b47ecf33d4e9a96e7fafa3c408767
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026370B2

反応ノート

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