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Hydrochloric Acid → {5-[2-(Thieno[3,2-d]pyrimidin-4-ylamino)-ethyl]-thiazol-2-yl}-carbamic acid phenyl ester

HRID 1818925
ノート
印刷プレビュー

反応式

HRID 1818925 の反応式
[C:1]([O:5][C:6](=[O:25])[NH:7][C:8]1[S:9][C:10]([CH2:13][CH2:14][NH:15][C:16]2[C:17]3[S:24][CH:23]=[CH:22][C:18]=3[N:19]=[CH:20][N:21]=2)=[CH:11][N:12]=1)([CH3:4])([CH3:3])C.Cl.C(N(CC)CC)C.ClC(O[C:38]1[CH:43]=CC=C[CH:39]=1)=O>O1CCOCC1.C1COCC1>[C:1]1([O:5][C:6](=[O:25])[NH:7][C:8]2[S:9][C:10]([CH2:13][CH2:14][NH:15][C:16]3[C:17]4[S:24][CH:23]=[CH:22][C:18]=4[N:19]=[CH:20][N:21]=3)=[CH:11][N:12]=2)[CH:3]=[CH:43][CH:38]=[CH:39][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 86603168{5-[2-(Thieno[3,2-d]pyrimidin-4-ylamino)-ethyl]-thiazol-2-yl}-carbamic acid tert-butyl ester

生成物 1

HCID 86603169{5-[2-(Thieno[3,2-d]pyrimidin-4-ylamino)-ethyl]-thiazol-2-yl}-carbamic acid phenyl ester

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
HCID 312751,4-Dioxane溶媒2 回

実験手順

To a suspension of compound 14.2 (23.7 mmol) in 1,4-dioxane (100 mL) was added HCl (70 mL of a 4.0 M in 1,4-dioxane) at 0° C. The reaction was allowed to warm to room temperature, stirred for 2 hours and concentrated to dryness to give a tan solid. The crude solid was suspended in THF (200 mL) and cooled to 0° C. Triethylamine (33 mL) was added followed by phenyl chloroformate (26.1 mmol). The reaction mixture was allowed to slowly warm to room temperature and stirred for 2 hours. Volatiles were removed under reduced pressure at room temperature, water was added and the solid collected by vacuum filtration. The solid was washed with ethyl ether and dried under vacuum to give {5-[2-(thieno[3,2-d]pyrimidin-4-ylamino)-ethyl]-thiazol-2-yl}-carbamic acid phenyl ester (compound 16.1) in 80% yield as a tan solid.

後処理

  1. concentrationconcentrated to dryness
  2. customto give a tan solid
  3. temperaturecooled to 0° C
  4. temperatureto slowly warm to room temperature
  5. stirringstirred for 2 hours
  6. customVolatiles were removed under reduced pressure at room temperature
  7. additionwater was added
  8. filtrationthe solid collected by vacuum filtration
  9. washThe solid was washed with ethyl ether
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-a798282908d04f38bbfbded3907c4112
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601725B2

反応ノート

読み込み中…

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