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Sodium Chloride → 2-(2,2-Difluoro-6-methoxybenzo[d][1,3]dioxol-5-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

HRID 1746055
ノート
印刷プレビュー

反応式

HRID 1746055 の反応式
[F:1][C:2]1([F:14])[O:6][C:5]2[CH:7]=[C:8]([O:12][CH3:13])[C:9](I)=[CH:10][C:4]=2[O:3]1.[Cl-].[Li+].C([Mg+])(C)C.[Cl-].C(O[B:26]1[O:30][C:29]([CH3:32])([CH3:31])[C:28]([CH3:34])([CH3:33])[O:27]1)(C)C.[NH4+].[Cl-].[Na+].[Cl-]>O1CCCC1.C(OCC)(=O)C>[F:1][C:2]1([F:14])[O:6][C:5]2[CH:7]=[C:8]([O:12][CH3:13])[C:9]([B:26]3[O:30][C:29]([CH3:32])([CH3:31])[C:28]([CH3:34])([CH3:33])[O:27]3)=[CH:10][C:4]=2[O:3]1
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

8

反応物 5

HCID 5234Sodium ChlorideHCID 25517Ammonium ChlorideHCID 50177412-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolaneHCID 904149712,2-Difluoro-5-iodo-6-methoxybenzo[d][1,3]dioxoleHCID 178461732HCID 178461732、化合物

生成物 1

HCID 904133722-(2,2-Difluoro-6-methoxybenzo[d][1,3]dioxol-5-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
2.5 °C

実験手順

2,2-Difluoro-5-iodo-6-methoxybenzo[d][1,3]dioxole (1.6 g, 5.0 mmol) was dissolved in dry tetrahydrofuran (15 mL), cooled to 0-5° C. and treated in portions with isopropylmagnesium lithium chloride (1.3 M; 4.1 mL, 5.3 mmol). After 50 min, 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.0 g, 5.4 mmol) was added and stirring was continued for 40 min at 15-20° C. The mixture was treated with saturated NH4Cl (10 mL) and then mixed with saturated NaCl (10 mL) and ethyl acetate (20 mL). The organic phase was washed with saturated NaCl (10 mL), dried (Na2SO4) and evaporated to give title compound as a thick oil which was used without further purification (1.4 g, 89%): 1H NMR (400 MHz, CDCl3) δ 7.35 (s, 1H), 6.65 (s, 1H), 3.81 (s, 3H), 1.34 (s, 12H); 19F NMR (376 MHz, CDCl3) δ −50.17 (s); EIMS m/z 314.

後処理

  1. waitwas continued for 40 min at 15-20° C
  2. washThe organic phase was washed with saturated NaCl (10 mL)
  3. dry with materialdried (Na2SO4)
  4. customevaporated

出典と根拠

ORDレコード
ord-874d5c44b6ca438b95ba84a71dbf649b
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09149038B2

反応ノート

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