ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dichloromethane → HCID 59560835、化合物

HRID 1176971
ノート
印刷プレビュー

反応式

HRID 1176971 の反応式
[CH2:1]([O:13][C:14]1[CH:15]=[C:16]([C:33]2([CH:39]([C:41]3[CH:46]=[CH:45][C:44]([I:47])=[CH:43][CH:42]=3)[OH:40])SCCCS2)[CH:17]=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C1C(=O)N(Br)C(=[O:51])C1.[O-]S([O-])=O.[Na+].[Na+].C(Cl)Cl>CC(C)=O.O.CC(C)=O>[CH2:1]([O:13][C:14]1[CH:15]=[C:16]([C:33](=[O:51])[C:39]([C:41]2[CH:46]=[CH:45][C:44]([I:47])=[CH:43][CH:42]=2)=[O:40])[CH:17]=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 24437Sodium SulfiteHCID 67184N-bromobutanimideHCID 72326541HCID 72326541、化合物

生成物 1

HCID 59560835HCID 59560835、化合物収率 25.4%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒
HCID 18366337
Propan-2-one--water (1/1)
溶媒

反応条件

温度
12.5 °C

実験手順

A solution of [2-(3,4-bis-dodecyloxy-phenyl)-[1,3]dithian-2-yl]-(4-iodo-phenyl)-methanol (JYC-II-020-A) (8.2 g, 10.3 mmol) in 400 mL of acetone was added dropwise to a solution of NBS (31.86 g, 17.9 mmol) in 3% water/acetone (v/v) at 0° C. The reaction mixture was stirred at 0-25° C. for 30 min. It was then poured into a saturated aqueous Na2SO3 solution (400 mL) and CH2Cl2 (400 mL) mixture. The resulting mixture was stirred at room temperature for additional 10 min. The organic layer was washed with H2O and dried over anhydrous MgSO4. The solvent was removed under reduced pressure. The crude product was recrystallized from hexanes. The product was further purified by column chromatography (silica gel, hexanes:dichloromethane=2:1 (v/v)) to give a light yellow solid (1.84 g, 25.4%). 1H NMR (300 MHz, CDCl3, δ): 7.85 (d, J=8.5 Hz, 2H), 7.65 (d, J=8.5 Hz, 2H), 7.53 (d, J=1.9 Hz, 1H), 7.38 (dd, J=8.5 Hz, 1.9 Hz, 1H), 6.83 (d, J=8.2 Hz, 1H), 4.04 (t, J=6.6 Hz, 2H), 4.03 (t, J=6.6 Hz, 2H), 1.76-1.86 (m, 4H), 1.20-1.51 (m, 36H), 0.86 (t, J=6.3 Hz, 6H). 13C {1H} NMR (75 MHz, CDCl3, δ): 193.77, 192.45, 155.19, 149.28, 138.17, 132.46, 130.90, 126.16, 125.47, 111.94, 111.46, 103.28, 69.21, 69.15, 32.00, 29.75, 29.70, 29.66, 29.45, 29.40, 29.10, 28.94, 26.06, 25.98, 22.78, 14.24. HRMS-EI (m/z): [M]+ calcd for C38H57IO4, 704.33016; found, 704.32941. Anal. calcd for C38H57IO4: C, 64.76; H, 8.15. Found: C, 64.81; H, 8.15.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for additional 10 min
  2. washThe organic layer was washed with H2O
  3. dry with materialdried over anhydrous MgSO4
  4. customThe solvent was removed under reduced pressure
  5. customThe crude product was recrystallized from hexanes
  6. customThe product was further purified by column chromatography (silica gel, hexanes:dichloromethane=2:1 (v/v))

出典と根拠

ORDレコード
ord-534cbc56053b4a86a512b8b865a4eff3
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842830B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート