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Trimethyl borate → 2-Fluoro-3-iodobenzyl alcohol

HRID 2096972
ノート
印刷プレビュー

反応式

HRID 2096972 の反応式
B(OC)(OC)OC.[F:8][C:9]1[C:17]([I:18])=[CH:16][CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12]>O1CCCC1>[F:8][C:9]1[C:17]([I:18])=[CH:16][CH:15]=[CH:14][C:10]=1[CH2:11][OH:12]
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 8470Trimethyl borateHCID 110545892-Fluoro-3-iodobenzoic acid

生成物 1

HCID 120412982-Fluoro-3-iodobenzyl alcohol収率 97%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Trimethyl borate (1.92 mL, 17.2 mmol) was added dropwise to a stirred solution of 2-fluoro-3-iodobenzoic acid (preparation 22b, 4.39 g, 16.5 mmol) in tetrahydrofuran (25 mL) at 0° C. and the mixture was stirred for a further 15 minutes at this temperature. Then borane-methyl sulfide complex (10 M, 4.4 mL, 44 mmol) in tetrahydrofuran (3 mL) was added dropwise to the mixture at 0° C. and the mixture was then allowed to warm to room temperature. After 1 hour, the mixture was carefully quenched by dropwise addition of methanol (10 mL). After stirring overnight, the mixture was concentrated in vacuo and ethyl acetate was added to the residue. The organic layer was washed with saturated aqueous potassium carbonate solution, brine, dried (MgSO4) and evaporated to give the title compound (4.03 g, 97%) as an oil.

後処理

  1. waitAfter 1 hour
  2. customthe mixture was carefully quenched by dropwise addition of methanol (10 mL)
  3. stirringAfter stirring overnight
  4. concentrationthe mixture was concentrated in vacuo and ethyl acetate
  5. additionwas added to the residue
  6. washThe organic layer was washed with saturated aqueous potassium carbonate solution, brine
  7. dry with materialdried (MgSO4)
  8. customevaporated

出典と根拠

ORDレコード
ord-a3299156cbdd4da2b0436335fbd7808c
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450341B2

反応ノート

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