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Trifluoroacetic acid → HCID 59471847、化合物

HRID 2204853
ノート
印刷プレビュー

反応式

HRID 2204853 の反応式
C(OC([N:8](C(OC(C)(C)C)=O)[C:9]1[N:10]=[CH:11][C:12]([C:26]2[CH:47]=[CH:46][C:29]([C:30]([N:32]3[CH2:38][CH2:37][CH2:36][N:35](C(OC(C)(C)C)=O)[CH2:34][CH2:33]3)=[O:31])=[CH:28][C:27]=2[C:48]#[N:49])=[N:13][C:14]=1[C:15]1[O:16][C:17]([C:20]2[S:21][CH:22]=[CH:23][C:24]=2[CH3:25])=[N:18][N:19]=1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl.C(#N)C.CO>[NH2:8][C:9]1[N:10]=[CH:11][C:12]([C:26]2[CH:47]=[CH:46][C:29]([C:30]([N:32]3[CH2:38][CH2:37][CH2:36][NH:35][CH2:34][CH2:33]3)=[O:31])=[CH:28][C:27]=2[C:48]#[N:49])=[N:13][C:14]=1[C:15]1[O:16][C:17]([C:20]2[S:21][CH:22]=[CH:23][C:24]=2[CH3:25])=[N:18][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

6

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 59472333HCID 59472333、化合物

生成物 1

HCID 59471847HCID 59471847、化合物収率 43.8%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane
溶媒

実験手順

tert-Butyl 4-[4-[5-[bis(tert-butoxycarbonyl)amino]-6-[5-(3-methyl-2-thienyl)-1,3,4-oxadiazol-2-yl]pyrazin-2-yl]-3-cyano-benzoyl]-1,4-diazepane-1-carboxylate (9.9 g, 11.32 mmol) was dissolved in anhydrous CH2Cl2 (100 mL) at room temperature and TFA (10 mL, 129.8 mmol) added. Additional TFA (10 mL, 129.8 mmol) was added and the reaction mixture stirred at room temperature for 3.5 h and then concentrated in vacuo. The material was dissolved in a mixture of acetonitrile and methanol (10; 1 mixture) and PS—HCO3 (5 eq) added. The mixture was stirred for 1 h at room temperature and then the resin removed by filtration and washed with acetonitrile and methanol. The filtrate was concentrated in vacuo and the residue recrystallised from acetonitrile. The isolated solid was washed with ether and dried to give the product as a yellow solid (2.41 g, 35% yield); 1H NMR (400 MHz, DMSO) d 1.76-1.84 (m, 2H), 2.67 (s, 3H), 2.88-2.93 (m, 4H), 3.42-3.44 (m, 2H), 3.67-3.74 (m, 2H), 7.2 (d, 1H), 7.84-7.87 (m, 1H), 7.89-7.99 (m, 1H), 8.04-8.09 (m, 2H) and 8.85 (s, 1H) ppm; MS (ES+) 487.26

後処理

  1. concentrationconcentrated in vacuo
  2. additionadded
  3. stirringThe mixture was stirred for 1 h at room temperature
  4. customthe resin removed by filtration
  5. washwashed with acetonitrile and methanol
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue recrystallised from acetonitrile
  8. washThe isolated solid was washed with ether
  9. customdried

出典と根拠

ORDレコード
ord-60613701dde249c6be1f1ffe43cd767a
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365557B2

反応ノート

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