Diisopropylethylamine → HCID 66618085、化合物

HRID 222157

反応式

HRID 222157 の反応式
C(S([C:11]1[C:12]2[CH:19]=[CH:18][N:17]([C@H:20]3[CH2:36][C@@H:23]4[O:24][CH:25]([C:28]5[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=5)[O:26][CH2:27][C@@H:22]4[CH2:21]3)[C:13]=2[N:14]=[CH:15][N:16]=1)(=O)=O)C1C=CC=CC=1.[NH2:37][C@H:38]1[C:46]2[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=2)[CH2:40][CH2:39]1.CCN(C(C)C)C(C)C>C(O)C>[C@H:38]1([NH:37][C:11]2[C:12]3[CH:19]=[CH:18][N:17]([C@H:20]4[CH2:36][C@@H:23]5[O:24][CH:25]([C:28]6[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=6)[O:26][CH2:27][C@@H:22]5[CH2:21]4)[C:13]=3[N:14]=[CH:15][N:16]=2)[C:46]2[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=2)[CH2:40][CH2:39]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2733933(R)-(-)-1-AminoindanHCID 58944569HCID 58944569、化合物

生成物 1

HCID 66618085HCID 66618085、化合物収率 73.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
110 °C

実験手順

In a 0.5-2 mL microwave vial, 4-(benzylsulfonyl)-7-[(4aS,6R,7aS)-2-(4-methoxyphenyl)hexahydrocyclopenta[d][1,3]dioxin-6-yl]-7H-pyrrolo[2,3-d]pyrimidine (100 mg, 0.198 mmol), (R)-(−)-1-aminoindan (0.127 mL, 0.989 mmol), and DIPEA (0.172 mL, 0.989 mol) were dissolved in ethanol (1.22 mL). The vial was sealed and heated to 110° C. overnight. The solution was then concentrated in vacuo and the resulting material was purified via silica gel chromatography eluting with a gradient of 20 to 50% EtOAc in hexanes to afford the product as an orange oil (70.0 mg, 73%). LC/MS: Rt=1.42 min, ES+ 483 (FA standard).

後処理

  1. customThe vial was sealed
  2. concentrationThe solution was then concentrated in vacuo
  3. customthe resulting material was purified via silica gel chromatography
  4. washeluting with a gradient of 20 to 50% EtOAc in hexanes

出典と根拠

ORDレコード
ord-b7523829933d4a34b95a71ab1911690c
出典データセット
uspto-grants-2012_06
特許番号
US08207177B2

関連ノート

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