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Tetrahydrofuran → HCID 18971050、化合物

HRID 2395202
ノート
印刷プレビュー

反応式

HRID 2395202 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][C:26]([F:38])([F:37])[C:27]([F:36])([F:35])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30])=[CH:19][CH:18]=2)=[CH:13][CH:12]=1.C(N(CC)CC)C.[O:46]1C[CH2:49][CH2:48][CH2:47]1.C(Cl)(=O)C=C>O>[C:47]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][C:26]([F:37])([F:38])[C:27]([F:35])([F:36])[C:28]([F:33])([F:34])[C:29]([F:30])([F:31])[F:32])=[CH:19][CH:18]=2)=[CH:15][CH:16]=1)(=[O:46])[CH:48]=[CH2:49]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 18971052HCID 18971052、化合物

生成物 1

HCID 18971050HCID 18971050、化合物収率 44.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In a flask whose content had been replaced with Ar, 1.5 g of 4-(8-hydroxyoctyloxy)-4'-[2-(perfluorobutyl)ethyloxy]biphenyl, 0.3 g of triethylamine, and 16 ml of tetrahydrofuran were placed. While this solution was being cooled with ice water, 0.3 g of acryloyl chloride was added dropwise. The reaction solution was allowed to warm up to room temperature, and was stirred for 3 hours. Thereafter, the reaction solution was poured into water and an organic layer was extracted with benzene. After the benzene layer was washed with water and dried over sodium sulfate anhydrous, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: benzene), and recrystallized from acetone to give 0.7 g of 4-[8-(acryloyloxy)octyloxy]-4'-[2-(perfluorobutyl)ethyloxy]biphenyl (Y: 44.4%). The purity of the compound thus obtained was 98.4% by GC; 99.4% by HPLC; and 1 spot by TLC. The phase transition temperature of the resultant compound was as shown in Table 2 below.

後処理

  1. additionwas added dropwise
  2. extractionan organic layer was extracted with benzene
  3. washAfter the benzene layer was washed with water
  4. dry with materialdried over sodium sulfate anhydrous
  5. distillationthe solvent was distilled away
  6. customThe residue was purified by silica gel column chromatography (eluent: benzene)
  7. customrecrystallized from acetone

出典と根拠

ORDレコード
ord-eb8b69166ff04960bed86e4711a1df8d
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05814378

反応ノート

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