Tetrahydrofuran → 2-(2-Chloro-1-chloromethyl-ethoxy)-6-(naphthalene-1-sulfonylmethyl)-phenylamine

HRID 33108노트

반응식

HRID 33108 반응식
[Cl:1][CH2:2][CH:3]([CH2:28][Cl:29])[O:4][C:5]1[C:6]([N+:25]([O-])=O)=[C:7]([CH2:11][S:12]([C:15]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=[CH:17][CH:16]=2)(=[O:14])=[O:13])[CH:8]=[CH:9][CH:10]=1.C1COCC1>[Pd].CO>[Cl:29][CH2:28][CH:3]([CH2:2][Cl:1])[O:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][S:12]([C:15]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=[CH:17][CH:16]=2)(=[O:13])=[O:14])[C:6]=1[NH2:25]

참가 물질

5

반응물 2

HCID 8028TetrahydrofuranHCID 597964381-[3-(2-Chloro-1-chloromethyl-ethoxy)-2-nitro-phenylmethanesulfonyl]-naphthalene

생성물 1

HCID 597964392-(2-Chloro-1-chloromethyl-ethoxy)-6-(naphthalene-1-sulfonylmethyl)-phenylamine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 1-[3-(2-chloro-1-chloromethyl-ethoxy)-2-nitro-phenylmethanesulfonyl]-naphthalene (3) (2.4 g, 5.3 mmoles) and 10% Pd/C in a 1:1 mixture of THF and methanol was hydrogenated on a Parr hydrogenator at 40 lb/in2 for 20 hours. The mixture was filtered through Celite. The filtrate was diluted with EtOAc, washed with water, dried over Na2SO4, and concentrated under vacuum to afford the title compound as an off white solid (2.02 g, 4.77 mmoles), identified by HNMR analysis.

후처리

  1. filtrationThe mixture was filtered through Celite
  2. additionThe filtrate was diluted with EtOAc
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-b07f7d877af1452ca4c32d8926e06992
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429582B2

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