2-Methyl-1-benzothiophene-7-carboxylic acid → HCID 58566649, 화합물

HRID 1876363노트

반응식

HRID 1876363 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

HCID 58566649HCID 58566649, 화합물수율 91.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e19d6285a0a54850b865c426b87ce4c1
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309600B2

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