Water → (4-Phenylsulfanylmethyl-phenyl)-methanol

HRID 1691344

반응식

HRID 1691344 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([S:13][CH2:14][C:15]2[CH:23]=[CH:22][C:18]([C:19](O)=[O:20])=[CH:17][CH:16]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.O>O1CCCC1>[C:7]1([S:13][CH2:14][C:15]2[CH:16]=[CH:17][C:18]([CH2:19][OH:20])=[CH:22][CH:23]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 8758244-[(Phenylsulfanyl)methyl]benzoic acidHCID 21226445Aluminium lithium hydride

생성물 1

HCID 59255239(4-Phenylsulfanylmethyl-phenyl)-methanol수율 42.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of lithium aluminum hydride (1.95 g, 51.3 mmol) in tetrahydrofuran (50 mL) was added dropwise a tetrahydrofuran solution of 4-phenylsulfanylmethyl-benzoic acid (5 g, 20.5 mmol) described in Manufacturing Example 206-1-1, which was stirred for 30 minutes at room temperature. This mixture was cooled with ice water, and water was carefully added. The mixture was filtered through a Celite bed, and the filtrate was combined. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (2.01 g). The title compound was used in the following reaction without any further purification.

후처리

  1. additionwas carefully added
  2. filtrationThe mixture was filtered through a Celite bed
  3. customThe organic layer was separated
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-a3d9974aedcb4b59af467e20b7fa59be
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153662B2

연결된 노트

불러오는 중…