Hydrochloric Acid → HCID 22250074, 화합물

HRID 889897노트

반응식

HRID 889897 반응식
C([O:3][C:4]([C:6]1[S:10][C:9]([C:11]2[S:19][C:18]3[C:13](=[N:14][CH:15]=[CH:16][C:17]=3[Cl:20])[CH:12]=2)=[N:8][C:7]=1[CH3:21])=[O:5])C.C1COCC1.[OH-].[K+].Cl>C(O)C>[Cl:20][C:17]1[CH:16]=[CH:15][N:14]=[C:13]2[CH:12]=[C:11]([C:9]3[S:10][C:6]([C:4]([OH:5])=[O:3])=[C:7]([CH3:21])[N:8]=3)[S:19][C:18]=12

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 69585794HCID 69585794, 화합물

생성물 1

HCID 22250074HCID 22250074, 화합물수율 72%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 15.2 g (46.2 mmol) 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-4-methyl-thiazole-5-carboxylic acid ethyl ester, 80 mL of THF and 20 mL of absolute ethanol was added (13 g, 231 mmol) freshly ground potassium hydroxide. The reaction was stirred at room temperature for sixteen hours. The reaction was cooled to 0° C. and the pH was adjusted to pH 3 with conc HCl. The resulting yellow precipitate was filtered and dried to give 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-4-methyl-thiazole-5-carboxylic acid (10.3 g) in 72% yield. C12H7N2O2S2: APCI m/z 310.2/312.2 (pos.); 1H NMR (d6-DMSO): δ 8.67 (d, 1H, J=5.0 Hz), 8.42 (s, 1H), 7.65 (d, 1H, J=5.0 Hz), 2.65 (s, 3H) ppm.

후처리

  1. temperatureThe reaction was cooled to 0° C.
  2. filtrationThe resulting yellow precipitate was filtered
  3. customdried

출처 및 근거

ORD 기록
ord-90d8a049298243a8bf7f56903cba1de3
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995171B2

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