2-Methyl-1-benzothiophene-7-carboxylic acid → HCID 58566649、化合物

HRID 1909520ノート

反応式

HRID 1909520 の反応式
[CH3:1][C:2]1[S:6][C:5]2[C:7]([C:11](O)=[O:12])=[CH:8][CH:9]=[CH:10][C:4]=2[CH:3]=1>O1CCCC1>[CH3:1][C:2]1[S:6][C:5]2[C:7]([CH2:11][OH:12])=[CH:8][CH:9]=[CH:10][C:4]=2[CH:3]=1

参加物

3

反応物 1

HCID 126239032-Methyl-1-benzothiophene-7-carboxylic acid

生成物 1

HCID 58566649HCID 58566649、化合物収率 91.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

The carboxylic acid (509) (0.240 g, 1.25 mmol) was dissolved in anhydrous tetrahydrofuran (12 mL) and cooled to 0° C. under nitrogen. BH3-tetrahydrofuran complex (3.12 mL, 3.12 mmol, 1.0 M in tetrahydrofuran) was added slowly. After the addition was complete, the solution was allowed to warm to room temperature and stirred for an additional 1 hour. The solution was cooled to 0° C. and quenched by the addition of methanol (5 mL) followed by a saturated sodium sulfate aqueous solution (5 mL). The mixture was diluted with ethyl acetate and washed with brine and dried over sodium sulfate, filtered, and concentrated in vacuo to provide (2-methylbenzo[b]thiophen-7-yl)methanol (510) (0.203 g, 91.2%) as a colorless oil.

後処理

  1. additionAfter the addition
  2. temperatureto warm to room temperature
  3. temperatureThe solution was cooled to 0° C.
  4. customquenched by the addition of methanol (5 mL)
  5. additionThe mixture was diluted with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a30dc115e41f4743a56461ba8e98d277
出典データセット
uspto-grants-2013_12
特許番号
US08598374B2

反応ノート

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