Ethyl 2-chloroacetoacetate → 5-Thiazolecarboxylic acid, 2-(3-cyano-4-(2-methylpropoxy)phenyl)-4-methyl-, ethyl ester

HRID 870881노트

반응식

HRID 870881 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH2:13][CH:14]([CH3:16])[CH3:15])[C:6](=[S:8])[NH2:7])#[N:2].[CH2:17]([O:19][C:20](=[O:26])[CH:21](Cl)[C:22]([CH3:24])=O)[CH3:18]>O>[C:1]([C:3]1[CH:4]=[C:5]([C:6]2[S:8][C:21]([C:20]([O:19][CH2:17][CH3:18])=[O:26])=[C:22]([CH3:24])[N:7]=2)[CH:9]=[CH:10][C:11]=1[O:12][CH2:13][CH:14]([CH3:16])[CH3:15])#[N:2]

참가 물질

4

반응물 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 117703963-Cyano-4-isobutoxybenzothioamide

생성물 1

HCID 98845495-Thiazolecarboxylic acid, 2-(3-cyano-4-(2-methylpropoxy)phenyl)-4-methyl-, ethyl ester수율 90.7%

시약·촉매·용매 1

HCID 962Water용매

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온도
25 °C

실험 절차

Water (30 mL) was placed into a round bottom flask and 3-cyano-4-isobutoxybenzothioamide (3.0 g) was added, followed by addition of ethyl-2-chloroacetoacetate (2.52 g). The mixture was heated to reflux and maintained until reaction completion. After the reaction was completed, the mass was cooled to about 25° C. and maintained for about 20 minutes. The mass was then filtered. The wet solid was dried at about 60° C. to a constant weight to yield 4.0 g of the title compound. Purity by HPLC: 95.74%.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperaturemaintained until reaction completion
  4. temperaturemaintained for about 20 minutes
  5. filtrationThe mass was then filtered
  6. customThe wet solid was dried at about 60° C. to a constant weight

출처 및 근거

ORD 기록
ord-3e36d188c1b34488a7d3f5995aee45dd
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969582B2

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