Hydrochloric Acid → HCID 59200469, 화합물

HRID 1685357노트

반응식

HRID 1685357 반응식
[F:1][C:2]1[C:3]([C:24]([O:26]C)=[O:25])=[N:4][CH:5]=[CH:6][C:7]=1[S:8][C:9]1[S:13][C:12]([NH:14][C:15]2[C:20]3[CH:21]=[CH:22][S:23][C:19]=3[CH:18]=[CH:17][N:16]=2)=[N:11][CH:10]=1.[OH-].[Na+].Cl>O>[F:1][C:2]1[C:3]([C:24]([OH:26])=[O:25])=[N:4][CH:5]=[CH:6][C:7]=1[S:8][C:9]1[S:13][C:12]([NH:14][C:15]2[C:20]3[CH:21]=[CH:22][S:23][C:19]=3[CH:18]=[CH:17][N:16]=2)=[N:11][CH:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59200415HCID 59200415, 화합물

생성물 1

HCID 59200469HCID 59200469, 화합물수율 62%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of methyl 3-fluoro-4-(2-(thieno[3,2-c]pyridin-4-ylamino)thiazol-5-ylthio)picolinate (3.13 g, 7.48 mmol) was treated with aqueous sodium hydroxide (1N, 12 mL, 12.0 mmol) and was stirred at room temperature for 2 hours. The reaction was then acidified to pH ˜6 with 10% aqueous HCl and then poured into water (300 mL) and allowed to sit overnight for complete precipitation. The solid was collected by filtration, washed with water and air dried to give the title material (1.86 g, 62%). 1H NMR (400 MHz, DMSO-d6) δ ppm: 12.24 (1H, s), 8.22 (1H, d, J=5.56 Hz), 8.18 (1H, d, J=5.05 Hz), 8.15 (1H, d, J=5.81 Hz), 7.90 (1H, s), 7.87 (1H, d, J=5.56 Hz), 7.69 (1H, d, J=5.56 Hz), 6.94 (1H, t, J=5.31 Hz). LC/MS (M+H)+: 405. HPLC ret. time (Condition I): 1.28 min.

후처리

  1. customto sit overnight for complete precipitation
  2. filtrationThe solid was collected by filtration
  3. washwashed with water and air
  4. customdried

출처 및 근거

ORD 기록
ord-43388e777b0a42fd89ed01ac40b3dc59
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148400B2

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