p-Anisoyl chloride → HCID 9886338, 화합물

HRID 2288585노트

반응식

HRID 2288585 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:13]3[S:14][CH:15]=[CH:16][C:12]=3[CH2:11][CH2:10][NH:9]2)=[CH:4][CH:3]=1.[CH3:17][O:18][C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[C:13]3[S:14][CH:15]=[CH:16][C:12]=3[CH2:11][CH2:10][N:9]2[C:23]([C:22]2[CH:26]=[CH:27][C:19]([O:18][CH3:17])=[CH:20][CH:21]=2)=[O:24])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 7477p-Anisoyl chlorideHCID 8471TriethylamineHCID 186996347-(4-Chlorophenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

생성물 1

HCID 9886338HCID 9886338, 화합물수율 91%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

7-(4-Chloro-phenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridin (100 mg) in toluene (20 ml), 4-methoxybenzoyl chloride (68.3 mg) and triethylamine (1 ml) were mixed and the mixture stirred at RT for 2 h. The reaction mixture was extracted once with NaOH (1 M) and once with water, the organic phase dried (MgSO4) and evaporated to dryness resulting in yellow oil which was purified on silica gel using methylene chloride/methanol 19/1 as eluent. The resulting oil was treated with abs ethanol resulting in precipitation of crystals. Yield 91%, m.p. 129.5-130.0 C. MS. M+=383.

후처리

  1. extractionThe reaction mixture was extracted once with NaOH (1 M) and once with water
  2. dry with materialthe organic phase dried (MgSO4)
  3. customevaporated to dryness
  4. customresulting in yellow oil which
  5. customwas purified on silica gel
  6. additionThe resulting oil was treated with abs ethanol resulting in precipitation of crystals

출처 및 근거

ORD 기록
ord-ef0b3deb5c2c417e812c25ff873d8406
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06090797

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