홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ammonium Chloride → 1-Benzofuran-5-ylmethanol

HRID 1478937
노트
인쇄 미리보기

반응식

HRID 1478937 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH:10]=[O:11])=[CH:9][C:4]=2[CH:3]=[CH:2]1.[BH4-].[Na+].[NH4+].[Cl-]>CO.C(OCC)(=O)C>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][OH:11])=[CH:9][C:4]=2[CH:3]=[CH:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 27738751-Benzofuran-5-carbaldehydeHCID 4311764Sodium borohydride

생성물 1

HCID 27951791-Benzofuran-5-ylmethanol수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 5-benzofurancarboxaldehyde (10 g, 68 mmol) in MeOH (40 mL) was cooled in an ice bath. NaBH4 (3.84 g, 102 mmol) was added over a period of 2 hr and stirring continued for 20 min. Saturated NH4Cl was added. The mixture was suspended in ethyl acetate (100 mL) and the solid was filtered off. The solution was concentrated, partitioned between ethyl acetate and brine, dried over anhydrous Na2SO4, concentrated and dried under high vacuum to furnish benzofuran-5-ylmethanol (10 g, 100%) as a solid, which was taken up in CH2Cl2 (60 mL) to which SOCl2 (5.9 mL, 81 mmol) was added at room temperature. The reaction mixture was stirred for 3 hr. The reaction mixture was diluted with CH2Cl2, washed with a saturated solution of NaHCO3, then brine, dried over anhydrous Na2SO4, and concentrated in vacuo to furnish 5-chloromethylbenzofuran (10 g, 90%) as an oil. This material was used without further purification to synthesize D-benzofurylalanine according to C. Behrens, Tetrahedron 56 (2000), 9443-9449.

후처리

  1. filtrationthe solid was filtered off
  2. concentrationThe solution was concentrated
  3. custompartitioned between ethyl acetate and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-f9b7be7a343b4e2da948bffc3ef74e4c
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403789B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트