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Hydrochloric Acid → HCID 10194952、化合物

HRID 1582138
ノート
印刷プレビュー

反応式

HRID 1582138 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][N:28]=1)[C:6]([NH:8][C:9]1[S:10][C:11]2[C:17]([CH:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)=[CH:16][CH:15]=[C:14]([O:24][CH3:25])[C:12]=2[N:13]=1)=[O:7].Cl.[C:30](OC(=O)C)(=[O:32])[CH3:31].C(=O)(O)[O-].[Na+]>C1COCC1.O.C(N(CC)CC)C>[C:30]([N:21]1[CH2:20][CH2:19][CH:18]([C:17]2[C:11]3[S:10][C:9]([NH:8][C:6](=[O:7])[C:5]4[CH:26]=[CH:27][N:28]=[C:3]([O:2][CH3:1])[CH:4]=4)=[N:13][C:12]=3[C:14]([O:24][CH3:25])=[CH:15][CH:16]=2)[CH2:23][CH2:22]1)(=[O:32])[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 227195582-methoxy-N-(4-methoxy-7-piperidin-4-yl-benzothiazol-2-yl)-isonicotinamide

生成物 1

HCID 10194952HCID 10194952、化合物収率 74.3%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8471Triethylamine溶媒

実験手順

To a solution of 0.07 g (0.16 mMol) 2-methoxy-N-(4-methoxy-7-piperidin-4-yl-benzothiazol-2-yl)-isonicotinamide 1:2 hydrochloride in 4 ml THF were added 0.049 ml triethyl amine. At 0° C. 0.018 ml (0.11 mMol) acetic anhydride was added dropwise and stirred for 1 h. Then a mixture of 5 ml sat. aqueous sodium bicarbonate and 10 ml water were added. This was extracted three times with 15 ml ethyl acetate, the combined organic phases were dried over sodium sulfate and evaporated to dryness in vacuo. One obtained 0.036 g (51%) N-[7-(1-acetyl-piperidin-4-yl)-4-methoxy-benzothiazol-2-yl]-2-methoxy-isonicotinamide as a white solid. F.p.: 242-244° C.

後処理

  1. customAt 0° C
  2. additionwere added
  3. extractionThis was extracted three times with 15 ml ethyl acetate
  4. dry with materialthe combined organic phases were dried over sodium sulfate
  5. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-e0aa20f9068c4a9bb5331ca4b055b8cf
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06734179B2

反応ノート

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