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Trimethyl orthoformate → HCID 72948500、化合物

HRID 921640
ノート
印刷プレビュー

反応式

HRID 921640 の反応式
[Cl:1][C:2]1[C:7]([N:8]2[CH2:13][CH2:12][C:11](=O)[CH2:10][CH2:9]2)=[CH:6][C:5]([C:15]#[N:16])=[CH:4][C:3]=1[NH:17][C:18]1[N:23]=[C:22]([N:24]([CH:34]2[CH2:36][CH2:35]2)CC2C=CC(OC)=CC=2)[C:21]2=[N:37][CH:38]=[C:39]([C:40]#[N:41])[N:20]2[N:19]=1.[F:42][C:43]1([F:48])[CH2:46][CH:45]([NH2:47])[CH2:44]1.C(OC)(OC)OC.C([BH3-])#N.[Na+]>CO.O1CCCC1.O>[Cl:1][C:2]1[C:7]([N:8]2[CH2:9][CH2:10][CH:11]([NH:47][CH:45]3[CH2:46][C:43]([F:48])([F:42])[CH2:44]3)[CH2:12][CH2:13]2)=[CH:6][C:5]([C:15]#[N:16])=[CH:4][C:3]=1[NH:17][C:18]1[N:23]=[C:22]([NH:24][CH:34]2[CH2:35][CH2:36]2)[C:21]2=[N:37][CH:38]=[C:39]([C:40]#[N:41])[N:20]2[N:19]=1
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 9005Trimethyl orthoformateHCID 5003444Sodium cyanoborohydrideHCID 225009513,3-Difluorocyclobutan-1-amineHCID 86708485HCID 86708485、化合物2 回

生成物 1

HCID 72948500HCID 72948500、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒
2 回
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a vial charged with 2-((2-chloro-5-cyano-3-(4-oxopiperidin-1-yl)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (Intermediate 13) (30 mg, 0.053 mmol) and 3,3-difluorocyclobutanamine (6.79 mg, 0.063 mmol) in methanol (132 μl) and tetrahydrofuran (132 μl) was added trimethyl orthoformate (58.4 μl, 0.528 mmol). The reaction mixture was stirred at room temperature. Sodium cyanoborohydride (6.64 mg, 0.106 mmol) was added and the reaction mixture was stirred at room temperature 6 h. The reaction mixture was diluted with water and methanol and filtered. The solid was taken up in DMF and partitioned between water and ethyl acetate. The aqueous layer was washed with ethyl acetate (3×). The combined organics were washed with 10% lithium chloride solution, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude material was taken forward as is.

後処理

  1. stirringthe reaction mixture was stirred at room temperature 6 h
  2. filtrationfiltered
  3. custompartitioned between water and ethyl acetate
  4. washThe aqueous layer was washed with ethyl acetate (3×)
  5. washThe combined organics were washed with 10% lithium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6be7fbc5d481466fa23d04a7b70160d5
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273057B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート