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Methanol → HCID 22671955, 화합물

HRID 1279610
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HRID 1279610 반응식
[C:1]1([S:7]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][C:12]=2N)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)[C:23]1[CH:30]=[CH:29][C:26]([CH:27]=[O:28])=[CH:25][CH:24]=1.[C:32]([BH3-])#[N:33].[Na+].[CH3:36][OH:37]>C(O)(=O)C>[C:1]1([S:7]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][C:12]=2[NH:33][CH2:32][C:23]2[CH:24]=[CH:25][C:26]([C:27]([O:37][CH3:36])=[O:28])=[CH:29][CH:30]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887Methanol2회HCID 12173TerephthalaldehydeHCID 5003444Sodium cyanoborohydrideHCID 16773163HCID 16773163, 화합물

생성물 1

HCID 22671955HCID 22671955, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 4-phenylsulfonylamino-3-aminobenzotrifluoride (100 mg; prepared in Reference Example 26.) and terephthal aldehyde acid methyl ester (78 mg) in MeOH (2 ml), acetic Acid (1.5 ml) was added. The mixture was stirred for 2 hours at room temperature. After stirring, a solution of sodium cyanoborohydride (30 mg) in MeOH (2 ml) was added. The mixture was stirred for 2 hours at room temperature. The reaction solution was extracted with H2O-AcOEt, washed, dried over, filtered and concentrated. The precipitate was washed with hexane to give the title compound (146 mg) having the following physical data.

후처리

  1. stirringAfter stirring
  2. stirringThe mixture was stirred for 2 hours at room temperature
  3. extractionThe reaction solution was extracted with H2O-AcOEt
  4. washwashed
  5. customdried over,
  6. filtrationfiltered
  7. concentrationconcentrated
  8. washThe precipitate was washed with hexane

출처 및 근거

ORD 기록
ord-cf5f60eb12044e5a91718a1c4c630019
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448290B1

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